CN107501037A - A kind of preparation method of diiodomethane - Google Patents
A kind of preparation method of diiodomethane Download PDFInfo
- Publication number
- CN107501037A CN107501037A CN201710807564.XA CN201710807564A CN107501037A CN 107501037 A CN107501037 A CN 107501037A CN 201710807564 A CN201710807564 A CN 201710807564A CN 107501037 A CN107501037 A CN 107501037A
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- CN
- China
- Prior art keywords
- diiodomethane
- preparation
- sodium iodide
- washing
- stratification
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- 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.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/20—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms
- C07C17/202—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms two or more compounds being involved in the reaction
- C07C17/208—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms two or more compounds being involved in the reaction the other compound being MX
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of diiodomethane, it is characterised in that：The preparation of diiodomethane is completed including diiodomethane synthetic reaction, washing and purification step；The advantage of the invention is that：The present invention passes through Reasonable adjustment production technology so that technological operation is simple, and improves product yield, meets the demand in market, improves the economic benefit and social benefit of enterprise.
Description
Technical field
The invention belongs to organic compound preparation method field, and in particular to a kind of preparation method of diiodomethane.
Background technology
Diiodomethane, molecular formula are CH2I2, and molecular weight is 267.87, achromaticity and clarification to faint yellow heavy liquid, as point
Reagent is analysed, is also used for organic synthesis；It is one of domestic and international bulk article, is widely used in organic synthesis, point of mineral
Analyse with separating, the measure of the identification of pyridine and refraction coefficient, be especially largely used to synthesize cyclopropane.At present, do not increase it is advanced
Equipment and in the case of not increasing operating personnel's technical requirements, the product yield synthesized is not high.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to now provide, a kind of technique is simple, synthesis yield it is high two
The preparation method of iodomethane.
To achieve the above object, the technical scheme is that：A kind of preparation method of diiodomethane, its innovative point exist
In：The preparation of diiodomethane is completed including diiodomethane synthetic reaction, washing and purification step, is comprised the following steps that：
（1）Diiodomethane synthetic reaction
Sodium iodide, dichloromethane and solvent dimethylformamide are mixed, the ratio of weight and number of sodium iodide and dichloromethane is 2:
1, sodium iodide and dimethylformamide ratio of weight and number are 1: 1.5-1.7, are stirred and heated to 90 DEG C, isothermal reaction 3-9 hours；
（2）Washing
A, hypo solution is added into reacted mixture, stirred, stratification, discard water layer；
B, clear water is added, stirs, stratification, discards water layer；
（3）It is refined
It is evaporated under reduced pressure, obtains diiodomethane finished product.
Beneficial effects of the present invention are as follows：The present invention passes through Reasonable adjustment production technology so that and technological operation is simple, and
Product yield is improved, meets the demand in market, improves the economic benefit and social benefit of enterprise.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
Embodiment 1
A kind of preparation method of diiodomethane, including diiodomethane synthetic reaction, washing and purification step complete diiodomethane
Prepare, comprise the following steps that：
（1）Diiodomethane synthetic reaction
Sodium iodide, dichloromethane and solvent dimethylformamide are mixed, the ratio of weight and number of sodium iodide and dichloromethane is 2:
1, sodium iodide and dimethylformamide ratio of weight and number are 1: 1.5, are stirred and heated to 90 DEG C, isothermal reaction 4 hours；
（2）Washing
A, hypo solution is added into reacted mixture, stirred, stratification, discard water layer；
B, clear water is added, stirs, stratification, discards water layer；
（3）It is refined
It is evaporated under reduced pressure, obtains diiodomethane finished product.
Embodiment 2
A kind of preparation method of diiodomethane, including diiodomethane synthetic reaction, washing and purification step complete diiodomethane
Prepare, comprise the following steps that：
（1）Diiodomethane synthetic reaction
Sodium iodide, dichloromethane and solvent dimethylformamide are mixed, the ratio of weight and number of sodium iodide and dichloromethane is 2:
1, sodium iodide and dimethylformamide ratio of weight and number are 1: 1.7, are stirred and heated to 90 DEG C, isothermal reaction 8 hours；
（2）Washing
A, hypo solution is added into reacted mixture, stirred, stratification, discard water layer；
B, clear water is added, stirs, stratification, discards water layer；
（3）It is refined
It is evaporated under reduced pressure, obtains diiodomethane finished product.
Embodiment 3
A kind of preparation method of diiodomethane, including diiodomethane synthetic reaction, washing and purification step complete diiodomethane
Prepare, comprise the following steps that：
（1）Diiodomethane synthetic reaction
Sodium iodide, dichloromethane and solvent dimethylformamide are mixed, the ratio of weight and number of sodium iodide and dichloromethane is 2:
1, sodium iodide and dimethylformamide ratio of weight and number are 1: 1.6, are stirred and heated to 90 DEG C, isothermal reaction 6 hours；
（2）Washing
A, hypo solution is added into reacted mixture, stirred, stratification, discard water layer；
B, clear water is added, stirs, stratification, discards water layer；
（3）It is refined
It is evaporated under reduced pressure, obtains diiodomethane finished product.
The present invention passes through Reasonable adjustment production technology so that technological operation is simple, and improves product yield, meets
The demand in market, improve the economic benefit and social benefit of enterprise.
Above-described embodiment is presently preferred embodiments of the present invention, is not the limitation to technical solution of the present invention, as long as
The technical scheme that can be realized on the basis of above-described embodiment without creative work, it is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (1)
- A kind of 1. preparation method of diiodomethane, it is characterised in that：It is complete including diiodomethane synthetic reaction, washing and purification step Into the preparation of diiodomethane, comprise the following steps that：（1）Diiodomethane synthetic reactionSodium iodide, dichloromethane and solvent dimethylformamide are mixed, the ratio of weight and number of sodium iodide and dichloromethane is 2: 1, sodium iodide and dimethylformamide ratio of weight and number are 1: 1.5-1.7, are stirred and heated to 90 DEG C, isothermal reaction 3-9 hours；（2）WashingA, hypo solution is added into reacted mixture, stirred, stratification, discard water layer；B, clear water is added, stirs, stratification, discards water layer；（3）It is refinedIt is evaporated under reduced pressure, obtains diiodomethane finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710807564.XA CN107501037A (en) | 2017-09-08 | 2017-09-08 | A kind of preparation method of diiodomethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710807564.XA CN107501037A (en) | 2017-09-08 | 2017-09-08 | A kind of preparation method of diiodomethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107501037A true CN107501037A (en) | 2017-12-22 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710807564.XA Pending CN107501037A (en) | 2017-09-08 | 2017-09-08 | A kind of preparation method of diiodomethane |
Country Status (1)
| Country | Link |
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| CN (1) | CN107501037A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112961029A (en) * | 2021-02-02 | 2021-06-15 | 浙江肯特催化材料科技有限公司 | Preparation method of diiodomethane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020529A (en) * | 2009-09-23 | 2011-04-20 | 天津市化学试剂研究所 | Method for preparing diiodomethane |
| CN106673954A (en) * | 2015-11-06 | 2017-05-17 | 南通德益化工有限公司 | Preparation method of diiodomethane |
-
2017
- 2017-09-08 CN CN201710807564.XA patent/CN107501037A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020529A (en) * | 2009-09-23 | 2011-04-20 | 天津市化学试剂研究所 | Method for preparing diiodomethane |
| CN106673954A (en) * | 2015-11-06 | 2017-05-17 | 南通德益化工有限公司 | Preparation method of diiodomethane |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112961029A (en) * | 2021-02-02 | 2021-06-15 | 浙江肯特催化材料科技有限公司 | Preparation method of diiodomethane |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171222 |
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