CN109096111A - A kind of synthetic method of chloro-methyl-chloroformate - Google Patents
A kind of synthetic method of chloro-methyl-chloroformate Download PDFInfo
- Publication number
- CN109096111A CN109096111A CN201811058095.7A CN201811058095A CN109096111A CN 109096111 A CN109096111 A CN 109096111A CN 201811058095 A CN201811058095 A CN 201811058095A CN 109096111 A CN109096111 A CN 109096111A
- Authority
- CN
- China
- Prior art keywords
- chloro
- methyl
- chloroformate
- synthetic method
- synthesis reactor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/02—Preparation of esters of carbonic or haloformic acids from phosgene or haloformates
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of synthetic method of chloro-methyl-chloroformate, methanol and phosgene are passed through reaction tower, and liquid flows in reserve tank after synthesis, and gas is collected by condenser；Nitrogen is passed into inside synthesis reactor from top and catches up with gas, catches up with gas from chlorine progress in bottom is secondary, then methylchloroformate is atomized；First high-pressure lamp is lighted, starting stirring and temperature control, methylchloroformate is sprayed from top and is entered in kettle, liquid methylchloroformate is added from bottom portion simultaneously, start return-flow system, circulating reflux simultaneously detects chloro-methyl-chloroformate changes of contents, is passed through nitrogen after the reaction was completed and carries out catching up with gas and be condensed, distilled in kettle, heavy distillat it is cooling chloro-methyl-chloroformate；The present invention promotes going on smoothly for reaction, operation of the present invention is simple using infrared ray, ultraviolet light and visible light auxiliary heating, good economy performance, great market potential, promotional value are high, can industrialized production, make product content not less than 98%, the quantity of other chlorides is no more than 0.0002%.
Description
Technical field
The present invention relates to pesticide synthesis technology fields, and in particular to a kind of synthetic method of chloro-methyl-chloroformate.
Background technique
Chloro-methyl-chloroformate, colourless liquid have stink, severe toxicity.Dissolve in a variety of organic solvents such as ethyl alcohol, ether.It is used as
The intermediate of medicine, pesticide, also makees military tear gas.
In Olofson, R.A. and Martz, the DE.3241568 (1983) of J.T is disclosed to be reacted with formaldehyde and phosgene
Method to prepare Lyu's acid adding chloro methyl esters, uses PhCH2Bu3When NCl is as catalyst, yield 42%；With [(Bu2N)2CCl]+
Cl-When as catalyst, yield be can be improved to 91.5%；But phosgene quite dangerous used is unsuitable for industrialized production, and institute
With expensive catalyst, it is not suitable for industrializing yet.
It is disclosed in Sekine, the JP08040986 (1996) of Yasuo et al. and uses ClCO2Me and SO2Cl2Reaction preparation
The method of chloro-methyl-chloroformate, but product does not separate.
It is disclosed in the DE.3826584 (1989) of MoqyorodiFerenc et al. logical using methylchloroformate and chlorine
Cross the method that liquid phase Light chlorimation prepares chloro-methyl-chloroformate, wherein use up as visible light, be passed through in reaction solution by control
The amount of chlorine, control conversion.When conversion ratio is 40%, the selectivity of chloro-methyl-chloroformate can reach 99.7%, and yield is
98%；When conversion ratio is 88%, the content of chloro-methyl-chloroformate is 70.5%, yield 61.9%, and dichloro- by-product is
29.6%, yield 26%；When conversion ratio is 96%, the content of chloro-methyl-chloroformate is 63.8%, yield 61.2%, two
Chloro by-product is 33.9%, yield 32.5%, and three chloro by-products contents are 2.4%, yield 23%.Liquid phase chlorination is anti-
Should by control conversion ratio, improve the content of chloro-methyl-chloroformate, production efficiency is lower, the yield of primary first-order equation less than 40%,
The rate of recovery of raw material needs more equipment.
Therefore, need a kind of high production efficiency, avoid that more chlorinations carry out, product and reactant it is segregative
The synthetic method of chloro-methyl-chloroformate.
Summary of the invention
To solve the above problems, the present invention is intended to provide a kind of high production efficiency, it is avoiding that more chlorinations carry out, produce
The synthetic method of object and the segregative chloro-methyl-chloroformate of reactant.
Purpose to realize the present invention, the technical solution adopted is that: a kind of synthetic method of chloro-methyl-chloroformate, the synthesis
Method the following steps are included:
1) synthesis of methylchloroformate: methanol is added in reaction tower by flowmeter, and phosgene passes through buffer and flowmeter
Into reaction tower, phosgene remains 1.05~1.1:1 to the molar ratio of methanol, and temperature is controlled at 35~40 DEG C, reacts 2~3h,
The content of methylchloroformate is more than 90% in Synthesis liquid at this time, and liquid flows in reserve tank for use, after gas is collected by condenser
Tower is destroyed into tail gas, cooling methylchloroformate liquid instills reserve tank；
The tail gas destroys the downstream connection hydrochloric acid absorption tower of tower, the downstream connection hydrochloric acid reserve tank of the hydrochloric acid absorption tower
With tail gas liberation port；
The tail gas, which destroys inside tower, phosgene decomposition catalyst；
2) synthesis of chloro-methyl-chloroformate: the nitrogen after dry removal of impurities is passed into inside synthesis reactor from top and is caught up with
30~60min of gas, then from bottom be passed through chlorine after dry removal of impurities carry out it is secondary catch up with 10~30min of gas, then step 1 is synthesized
Methylchloroformate is delivered to atomizer and is atomized；
First the high-pressure lamp being arranged in inside synthesis reactor is lighted, starting stirring starts program-controlled thermostat A and program-controlled thermostat
B controls the temperature of synthesis reactor upper and lower part respectively, then from top by the methylchloroformate being atomized by sprayer it is spraying into
Enter into synthesis reactor, and simultaneously from synthesis reactor bottom be added liquid methylchloroformate, start return-flow system, circulating reflux 1~
For 24 hours, the changes of contents of flow liquid detection chloro-methyl-chloroformate is fetched at interval of 30~60min, it is constant to chloro-methyl-chloroformate content
When stop reaction；
The program-controlled thermostat A connects the upper half of synthesis reactor by heat preservation connecting tube, and program-controlled thermostat B is connected by heat preservation
The lower half of adapter tube connection synthesis reactor；
Thermal insulation board is provided in the middle part of the synthesis reactor, wherein gas-liquid hole is provided on thermal insulation board；
The return-flow system includes synthesis reactor, reflux cycle pump and reflux atomizer, wherein reflux atomizer and spraying
Device is symmetrical arranged；
The chlorine for participating in reaction and methylchloroformate total moles ratio are 1:3.5~5, wherein the chloromethane being atomized
The molar ratio of sour methyl esters and synthesis reactor bottom liquid methylchloroformate is 1~1.5:2~4；
3) separation of chloro-methyl-chloroformate: after the reaction was completed, stop heating, stop stirring, stop reflux, be passed through high temperature
Under nitrogen carry out catching up with 10~30min of gas and be condensed using condenser, condensate liquid is applied in atomizer, controls program-controlled perseverance
Warm slot A and program-controlled thermostat B distills the raising of synthesis reactor temperature, is condensed and is applied in atomizer using condenser, steams
Evaporate interprocedual every 30~45min take solid detection chloro-methyl-chloroformate changes of contents, when its content is constant, cool to
It saves at 2~8 DEG C to get chloro-methyl-chloroformate.
Preferably, condenser is divided into condenser A and condenser B in the synthetic method step 1, wherein cold in condenser A
Source temperature is set as 65~70 DEG C, and the sink temperature of condenser B is set as 10~60 DEG C.
Preferably, the gas of gas is caught up with to pass through removal of impurities drying device in the synthetic method step 2, wherein removal of impurities is dry
Active carbon and active molecular sieve are filled with inside dry device, wherein the both ends of active molecular sieve are arranged in active carbon.
Preferably, the synthetic method step 2 mesohigh lamp is set as infrared high-voltage lamp or ultraviolet light high-pressure lamp or can
Light-exposed high-pressure lamp, wherein high-pressure lamp is arranged in quartz glass tube；
The high-pressure lamp is arranged on the inner wall of synthesis reactor, wherein the number of high-pressure lamp is set as 4~8.
Preferably, program-controlled thermostat A is identical as the temperature of the synthesis reactor upper half in the synthetic method step 2, is set as
75~105 DEG C；
Program-controlled thermostat B is identical as the temperature of the lower half of synthesis reactor, is set as 20~70 DEG C.
Preferably, the nitrogen of gas is caught up with to first pass through dry exclusion device, the temperature setting of nitrogen in the synthetic method step 3
It is 75~105 DEG C.
Preferably, condenser is arranged at the upper outlet of synthesis reactor in the synthetic method step 3, the condensation of condenser
Temperature setting is 20~70 DEG C.
Preferably, the temperature phase in the synthetic method step 3 in program-controlled thermostat A, program-controlled thermostat B and synthesis reactor
Together, 75~105 DEG C are disposed as.
The principle of the present invention are as follows: methanol and phosgene reaction generate methylchloroformate, chemical equation are as follows:
Methylchloroformate and chlorine generate chloro-methyl-chloroformate, chemical equation under high-pressure lamp effect are as follows:
The invention has the benefit that the synthetic method strict control reaction temperature of chloro-methyl-chloroformate of the present invention, science
Various raw materials are matched, promotes rapid reaction to carry out by the way of spraying and circulating reflux, and improve product purity, has avoided
Noxious material discharge, it is environmental-friendly, it assists heating using infrared ray, ultraviolet light and visible light, promotes going on smoothly for reaction, this
Invent easy to operate, good economy performance, great market potential, promotional value is high, can industrialized production, contain chloro-methyl-chloroformate product
Amount is not less than 98%, and the quantity of other chlorides is no more than 0.0002%.
Detailed description of the invention
Fig. 1 is the flowage structure simplified schematic diagram of the synthetic method of chloro-methyl-chloroformate of the present invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
Embodiment 1
As shown in Figure 1, the technical solution adopted by the present invention are as follows: a kind of synthetic method of chloro-methyl-chloroformate, the synthesis
Method the following steps are included:
1) synthesis of methylchloroformate: methanol is added in reaction tower by flowmeter, and phosgene passes through buffer and flowmeter
Into reaction tower, phosgene remains 1.05:1 to the molar ratio of methanol, and temperature controls at 35~40 DEG C, reacts 2~3h, close at this time
Content at methylchloroformate in liquid is more than 90%, and liquid flows in reserve tank for use, and gas enters tail after being collected by condenser
Gas destroys tower, and cooling methylchloroformate liquid instills reserve tank；
The tail gas destroys the downstream connection hydrochloric acid absorption tower of tower, the downstream connection hydrochloric acid reserve tank of the hydrochloric acid absorption tower
With tail gas liberation port；
The tail gas, which destroys inside tower, phosgene decomposition catalyst；
2) synthesis of chloro-methyl-chloroformate: the nitrogen after dry removal of impurities is passed into inside synthesis reactor from top and is caught up with
Gas 45min, then be passed through the chlorine after dry removal of impurities from bottom and carry out secondary catching up with gas 15min, then the chloro-carbonic acid first that step 1 is synthesized
Ester is delivered to atomizer and is atomized；
First the high-pressure lamp being arranged in inside synthesis reactor is lighted, starting stirring starts program-controlled thermostat A and program-controlled thermostat
B controls the temperature of synthesis reactor upper and lower part respectively, then from top by the methylchloroformate being atomized by sprayer it is spraying into
Enter into synthesis reactor, and simultaneously from synthesis reactor bottom be added liquid methylchloroformate, start return-flow system, circulating reflux 1~
For 24 hours, the changes of contents that flow liquid detection chloro-methyl-chloroformate is fetched at interval of 30min, stops when chloro-methyl-chloroformate content is constant
Only react；
The program-controlled thermostat A connects the upper half of synthesis reactor by heat preservation connecting tube, and program-controlled thermostat B is connected by heat preservation
The lower half of adapter tube connection synthesis reactor；
Thermal insulation board is provided in the middle part of the synthesis reactor, wherein gas-liquid hole is provided on thermal insulation board；
The return-flow system includes synthesis reactor, reflux cycle pump and reflux atomizer, wherein reflux atomizer and spraying
Device is symmetrical arranged；
The chlorine for participating in reaction and methylchloroformate total moles ratio are 1:4.5, wherein the chloro-carbonic acid first being atomized
The molar ratio of ester and synthesis reactor bottom liquid methylchloroformate is 1.5:3；
3) separation of chloro-methyl-chloroformate: after the reaction was completed, stop heating, stop stirring, stop reflux, be passed through high temperature
Under nitrogen carry out catching up with gas 30min and be condensed using condenser, condensate liquid is applied in atomizer, controls program-controlled thermostat
A and program-controlled thermostat B distills the raising of synthesis reactor temperature, is condensed and is applied in atomizer using condenser, distilled
Journey interval 30min takes the changes of contents of solid detection chloro-methyl-chloroformate to cool when its content is constant at 2~8 DEG C
It saves to get chloro-methyl-chloroformate.
Further, condenser is divided into condenser A and condenser B in the synthetic method step 1, wherein in condenser A
Sink temperature is set as 65 DEG C, and the sink temperature of condenser B is set as 20 DEG C.
Further, the gas of gas is caught up with to pass through removal of impurities drying device in the synthetic method step 2, wherein removal of impurities
Active carbon and active molecular sieve are filled with inside drying device, wherein the both ends of active molecular sieve are arranged in active carbon.
Further, the synthetic method step 2 mesohigh lamp be set as infrared high-voltage lamp or ultraviolet light high-pressure lamp or
Visible light high-pressure lamp, wherein high-pressure lamp is arranged in quartz glass tube；
The high-pressure lamp is arranged on the inner wall of synthesis reactor, wherein the number of high-pressure lamp is set as 4~8.
Further, program-controlled thermostat A is identical as the temperature of the synthesis reactor upper half in the synthetic method step 2, setting
It is 75 DEG C；
Program-controlled thermostat B is identical as the temperature of the lower half of synthesis reactor, is set as 30 DEG C.
Further, the nitrogen of gas is caught up with to first pass through dry exclusion device in the synthetic method step 3, the temperature of nitrogen is set
It is set to 75 DEG C.
Further, condenser is arranged at the upper outlet of synthesis reactor in the synthetic method step 3, condenser it is cold
Solidifying temperature setting is 30 DEG C.
Further, the temperature phase in the synthetic method step 3 in program-controlled thermostat A, program-controlled thermostat B and synthesis reactor
Together, 75 DEG C are disposed as.
Wherein, the purity of chloro-methyl-chloroformate product is not less than 98%；
Wherein, the quantity of other chlorides is no more than 0.0002%.
In the present invention, the synthetic method strict control reaction temperature of chloro-methyl-chloroformate of the present invention, scientific matching are various
Raw material promotes rapid reaction to carry out, and improves product purity by the way of spraying and circulating reflux, and noxious material is avoided to arrange
It puts, it is environmental-friendly, it assists heating using infrared ray, ultraviolet light and visible light, promotes going on smoothly for reaction, operation of the present invention
Simply, good economy performance, great market potential, promotional value is high, can industrialized production.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of synthetic method of chloro-methyl-chloroformate, it is characterised in that: the synthetic method the following steps are included:
1) synthesis of methylchloroformate: methanol is added in reaction tower by flowmeter, and phosgene is entered by buffer and flowmeter
Reaction tower, phosgene remain 1.05~1.1:1 to the molar ratio of methanol, and temperature is controlled at 35~40 DEG C, react 2~3h, at this time
The content of methylchloroformate is more than 90% in Synthesis liquid, and liquid flows in reserve tank for use, and gas enters after being collected by condenser
Tail gas destroys tower, and cooling methylchloroformate liquid instills reserve tank；
The tail gas destroys the downstream connection hydrochloric acid absorption tower of tower, the downstream connection hydrochloric acid reserve tank and tail of the hydrochloric acid absorption tower
Gas liberation port；
The tail gas, which destroys inside tower, phosgene decomposition catalyst；
2) synthesis of chloro-methyl-chloroformate: the nitrogen after dry removal of impurities is passed into from top and carries out catching up with gas 30 inside synthesis reactor
~60min, then be passed through the chlorine after dry removal of impurities from bottom and carry out secondary catching up with 10~30min of gas, then the chloromethane that step 1 is synthesized
Sour methyl esters is delivered to atomizer and is atomized；
First the high-pressure lamp being arranged in inside synthesis reactor is lighted, starting stirring starts program-controlled thermostat A and program-controlled thermostat B points
Not Kong Zhi synthesis reactor upper and lower part temperature, then entered by spraying from top by the methylchloroformate being atomized by sprayer
In synthesis reactor, and liquid methylchloroformate is added from synthesis reactor bottom simultaneously, starts return-flow system, circulating reflux 1~for 24 hours, often
30~60min of interval fetches the changes of contents of flow liquid detection chloro-methyl-chloroformate, stops when chloro-methyl-chloroformate content is constant
Reaction；
The program-controlled thermostat A connects the upper half of synthesis reactor by heat preservation connecting tube, and program-controlled thermostat B passes through heat preservation connecting tube
Connect the lower half of synthesis reactor；
Thermal insulation board is provided in the middle part of the synthesis reactor, wherein gas-liquid hole is provided on thermal insulation board；
The return-flow system includes synthesis reactor, reflux cycle pump and reflux atomizer, wherein reflux atomizer and sprayer pair
Claim setting；
The chlorine for participating in reaction and methylchloroformate total moles ratio are 1:3.5~5, wherein the chloro-carbonic acid first being atomized
The molar ratio of ester and synthesis reactor bottom liquid methylchloroformate is 1~1.5:2~4；
3) separation of chloro-methyl-chloroformate: after the reaction was completed, stop heating, stop stirring, stop reflux, be passed through under high temperature
Nitrogen is carried out catching up with 10~30min of gas and be condensed using condenser, and condensate liquid is applied in atomizer, controls program-controlled thermostat
A and program-controlled thermostat B distills the raising of synthesis reactor temperature, is condensed and is applied in atomizer using condenser, distilled
30~45min of journey interval takes the changes of contents of solid detection chloro-methyl-chloroformate to cool when its content is constant to 2~8
It saves at DEG C to get chloro-methyl-chloroformate.
2. a kind of synthetic method of chloro-methyl-chloroformate according to claim 1, it is characterised in that: the synthetic method step
Condenser is divided into condenser A and condenser B in rapid 1, wherein sink temperature is set as 65~70 DEG C in condenser A, condenser B
Sink temperature be set as 10~60 DEG C.
3. a kind of synthetic method of chloro-methyl-chloroformate according to claim 1, it is characterised in that: the synthetic method step
The gas of gas is caught up with to pass through removal of impurities drying device in rapid 2, wherein to be filled with active carbon and activity point inside removal of impurities drying device
Son sieve, wherein the both ends of active molecular sieve are arranged in active carbon.
4. a kind of synthetic method of chloro-methyl-chloroformate according to claim 1, it is characterised in that: the synthetic method step
Rapid 2 mesohigh lamp is set as infrared high-voltage lamp or ultraviolet light high-pressure lamp or visible light high-pressure lamp, wherein high-pressure lamp is arranged in stone
In English glass tube；
The high-pressure lamp is arranged on the inner wall of synthesis reactor, wherein the number of high-pressure lamp is set as 4~8.
5. a kind of synthetic method of chloro-methyl-chloroformate according to claim 1, it is characterised in that: the synthetic method step
Program-controlled thermostat A is identical as the temperature of the synthesis reactor upper half in rapid 2, is set as 75~105 DEG C；
Program-controlled thermostat B is identical as the temperature of the lower half of synthesis reactor, is set as 20~70 DEG C.
6. a kind of synthetic method of chloro-methyl-chloroformate according to claim 1, it is characterised in that: the synthetic method step
The nitrogen of gas is caught up with to first pass through dry exclusion device in rapid 3, the temperature setting of nitrogen is 75~105 DEG C.
7. a kind of synthetic method of chloro-methyl-chloroformate according to claim 1, it is characterised in that: the synthetic method step
Condenser is arranged at the upper outlet of synthesis reactor in rapid 3, and the condensation temperature of condenser is set as 20~70 DEG C.
8. a kind of synthetic method of chloro-methyl-chloroformate according to claim 1, it is characterised in that: the synthetic method step
Program-controlled thermostat A, program-controlled thermostat B are identical with the temperature in synthesis reactor in rapid 3, are disposed as 75~105 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811058095.7A CN109096111A (en) | 2018-09-11 | 2018-09-11 | A kind of synthetic method of chloro-methyl-chloroformate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811058095.7A CN109096111A (en) | 2018-09-11 | 2018-09-11 | A kind of synthetic method of chloro-methyl-chloroformate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109096111A true CN109096111A (en) | 2018-12-28 |
Family
ID=64865944
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811058095.7A Pending CN109096111A (en) | 2018-09-11 | 2018-09-11 | A kind of synthetic method of chloro-methyl-chloroformate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109096111A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111957277A (en) * | 2020-08-24 | 2020-11-20 | 宜都市友源实业有限公司 | Production system and method for continuous chlorination of chloromethyl chloroformate |
| CN112300001A (en) * | 2020-11-10 | 2021-02-02 | 宁夏瑞泰科技股份有限公司 | Production method for co-production of ethyl chloroformate and ethyl chloride |
| CN112552176A (en) * | 2020-12-09 | 2021-03-26 | 安徽广信农化股份有限公司 | Synthesis process of methyl chloroformate |
| CN113527102A (en) * | 2021-07-20 | 2021-10-22 | 安徽东至广信农化有限公司 | Synthetic method of methyl chloroformate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2108961A (en) * | 1981-11-10 | 1983-05-25 | Poudres & Explosifs Ste Nale | Preparation of chloromethyl chloroformate from formaldehyde and phosgene |
| US20040152911A1 (en) * | 2003-02-05 | 2004-08-05 | Bowman Mark P | Method for purifying chloromethyl chloroformate |
| CN1648118A (en) * | 2004-01-19 | 2005-08-03 | 上海康鸣高科技有限公司 | Gas phase chlorination method and device for preparing chloro-formic acid-1-chloro-formic ester |
| CN102399149A (en) * | 2011-09-07 | 2012-04-04 | 扬州三友合成化工有限公司 | Preparation method of antiviral drug tenofovir disoproxil fumarate intermediate chloromethyl isopropyl carbonate |
| CN105001086A (en) * | 2015-06-29 | 2015-10-28 | 安徽广信农化股份有限公司 | Synthetic method of methylclhlorofonmate |
-
2018
- 2018-09-11 CN CN201811058095.7A patent/CN109096111A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2108961A (en) * | 1981-11-10 | 1983-05-25 | Poudres & Explosifs Ste Nale | Preparation of chloromethyl chloroformate from formaldehyde and phosgene |
| US20040152911A1 (en) * | 2003-02-05 | 2004-08-05 | Bowman Mark P | Method for purifying chloromethyl chloroformate |
| CN1648118A (en) * | 2004-01-19 | 2005-08-03 | 上海康鸣高科技有限公司 | Gas phase chlorination method and device for preparing chloro-formic acid-1-chloro-formic ester |
| CN102399149A (en) * | 2011-09-07 | 2012-04-04 | 扬州三友合成化工有限公司 | Preparation method of antiviral drug tenofovir disoproxil fumarate intermediate chloromethyl isopropyl carbonate |
| CN105001086A (en) * | 2015-06-29 | 2015-10-28 | 安徽广信农化股份有限公司 | Synthetic method of methylclhlorofonmate |
Non-Patent Citations (7)
| Title |
|---|
| FOLKMANN M, LUND F J.: "Acyloxymethyl Carbonochloridates. New Intermediates in Prodrug Synthesis", 《 SYNTHESIS》 * |
| 刘海望编: "《建筑工程设计》", 31 October 2008, 华中科技大学出版社 * |
| 卫月琴主编: "《有机化学基础》", 31 October 2013, 中医药出版社 * |
| 莫畏等编著: "《钛冶金》", 30 June 1979, 冶金工业出版社 * |
| 董岩: "氯化氯甲酸酯的制备方法", 《天津化工》 * |
| 陈仁学主编: "《化学反应工程与反应器》", 31 July 1988, 国防工业出版社 * |
| 黄德丰等编: "《化工常见故障排除法》", 31 December 1992, 湖南科学技术出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111957277A (en) * | 2020-08-24 | 2020-11-20 | 宜都市友源实业有限公司 | Production system and method for continuous chlorination of chloromethyl chloroformate |
| CN112300001A (en) * | 2020-11-10 | 2021-02-02 | 宁夏瑞泰科技股份有限公司 | Production method for co-production of ethyl chloroformate and ethyl chloride |
| CN112552176A (en) * | 2020-12-09 | 2021-03-26 | 安徽广信农化股份有限公司 | Synthesis process of methyl chloroformate |
| CN112552176B (en) * | 2020-12-09 | 2023-04-11 | 安徽广信农化股份有限公司 | Synthesis process of methyl chloroformate |
| CN113527102A (en) * | 2021-07-20 | 2021-10-22 | 安徽东至广信农化有限公司 | Synthetic method of methyl chloroformate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109096111A (en) | A kind of synthetic method of chloro-methyl-chloroformate | |
| CN100532338C (en) | Method for producing benzyl chloride compound | |
| CN107473949A (en) | A kind of synthesis technique of the pentanone of 3,5 dichloro 2 | |
| CN104876839A (en) | Process for preparing p-toluenesulfonic acid through gas phase SO3 film sulfonation | |
| CN109438204A (en) | Continuous flow reacts the method for preparing the chloro- 1- acetyl group cyclopropylamine of 1- | |
| CN105026365B (en) | Urea synthesis method and equipment | |
| CN108409526A (en) | A kind of monochloro methane production energy-saving system and method | |
| CN112010770A (en) | Novel production method of glycine ethyl ester hydrochloride | |
| CN103864615A (en) | Method for preparing ethyl trifluoroacetate through continuous non-catalytic method | |
| CN109053361A (en) | For reducing the method for impurity dichloro-benzenes in benzene chloride production technique | |
| CN105601520B (en) | A kind of nitromethane synthesis and product separator | |
| CN208741966U (en) | A kind of processing system of acrylonitrile recycling tower bottoms | |
| CN101357877A (en) | Method for preparing dibromomethane and methylene chlorobromide by one-pot | |
| CN101747176A (en) | Method for preparation of trifluoro acetyl chloride with trifluoroethane chlorinated mixture | |
| CN103539763A (en) | Reaction separation coupling technology for continuously preparing epoxy chloropropane from dichloropropanol | |
| CN108586399A (en) | A kind of synthetic method of Fei Luokao former times | |
| CN105366692B (en) | A kind of high purity liquid HCN and system | |
| CN108084001A (en) | A kind of synthetic method of improved 1- acetyl-1-chlorcyclopropanes | |
| ES2837130A2 (en) | Method and device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof | |
| CN103408413B (en) | Method for preparing deuterated chloroform by using hexachloroacetone as intermediate | |
| CN109096206A (en) | A kind of method of acidity photocatalytic method synthesis carbendazim | |
| CN112321462B (en) | Method for synthesizing chlorosulfonyl isocyanate by continuous method | |
| CN110963884B (en) | Preparation method of 1,1,1, 2-tetrachloro-2, 2-difluoroethane | |
| CN109265331A (en) | A kind of preparation process of benzophenone | |
| CN110372462B (en) | Continuous synthesis-purification integrated device and continuous reaction system comprising same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181228 |