CN104649866A - Safe, reliable and low-cost preparation method of 9-fluorenylmethanol - Google Patents
Safe, reliable and low-cost preparation method of 9-fluorenylmethanol Download PDFInfo
- Publication number
- CN104649866A CN104649866A CN201310593957.7A CN201310593957A CN104649866A CN 104649866 A CN104649866 A CN 104649866A CN 201310593957 A CN201310593957 A CN 201310593957A CN 104649866 A CN104649866 A CN 104649866A
- Authority
- CN
- China
- Prior art keywords
- preparation
- cost
- suction filtration
- fluorenylmethanol
- safe
- 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
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/36—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2603/00—Systems containing at least three condensed rings
- C07C2603/02—Ortho- or ortho- and peri-condensed systems
- C07C2603/04—Ortho- or ortho- and peri-condensed systems containing three rings
- C07C2603/06—Ortho- or ortho- and peri-condensed systems containing three rings containing at least one ring with less than six ring members
- C07C2603/10—Ortho- or ortho- and peri-condensed systems containing three rings containing at least one ring with less than six ring members containing five-membered rings
- C07C2603/12—Ortho- or ortho- and peri-condensed systems containing three rings containing at least one ring with less than six ring members containing five-membered rings only one five-membered ring
- C07C2603/18—Fluorenes; Hydrogenated fluorenes
Abstract
The invention relates to a safe, reliable and low-cost preparation method of 9-fluorenylmethanol. The preparation method comprises the following steps: (1) adding ethyl formate and fluorene into a reaction vessel, starting to stir, heating until system temperature reaches 40-90 DEG C; (2) adding sodium methylate in batches, releasing heat, generating bubbles, slowing adding, heating to reflux after addition, controlling temperature to 45-95 DEG C, keeping warm and reacting, and carrying out TLC point-plate tracking until the reaction is completely finished; and (3) cooling, carrying out suction filtration, adding mother liquor into a formaldehyde aqueous solution and stirring to form a solid, carrying out suction filtration, adding the solid, washing and draining, and recrystallizing by using petroleum ether with high boiling point so as to obtain 9-fluorenylmethanol. By using sodium methylate, the preparation method is economic, is convenient to operate and is safe. By using ethyl formate, reaction system is minimized, and cost is saved. By changing paraformaldehyde into the formaldehyde aqueous solution, cost is saved, and the preparation method is convenient to operate. The preparation method is simple, and has advantages of short production time, high production efficiency, high yield and low production cost.
Description
Technical field
The invention belongs to polyester art, especially a kind of based on safety reliable 9-Lumefantrine preparation method.
Background technology
9-Lumefantrine, English name: 9-Fluorenylmethanol, molecular formula: C
14h
12o, molecular weight: 196.25, becomes white or light yellow crystalline powder, as the very important chemical intermediate of one, increasingly extensive in the application in the fields such as pharmacy, functional pigmented and polymer.Its content of 9-Lumefantrine preparation method of the prior art is up to 98.3% (HPLC), but productive rate is high not enough, only has 36.7%, and preparation cost is higher.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of based on safety reliable 9-Lumefantrine preparation method, this preparation method is simple, the production time is short, production efficiency is high, productive rate is high, production cost is lower.
The present invention solves its technical problem and is achieved through the following technical solutions:
A kind of based on safety reliable 9-Lumefantrine preparation method, the step of its preparation method is:
(1), in reactor add ethyl formate, fluorenes, start stirring, be warming up to system temperature in 40-90 DEG C;
(2), in batches add sodium methylate, heat release, and have bubble to produce, slowly add, finish, be warming up to backflow, temperature controls at 45-95 DEG C, insulation reaction, and TLC point plate tracks to and reacts completely;
(3), lower the temperature, suction filtration, mother liquor adds formalin and stirs out solid, suction filtration, and solid is drained after adding washing, then uses high point petroleum ether recrystallization to obtain 9-Lumefantrine.
Advantage of the present invention and beneficial effect are:
The present invention uses sodium ethylate to make catalyzer and now changes sodium methylate into, economical, handled easily, safety.The present invention uses ethyl formate, and reaction system is reduced, cost-saving.The present invention changes paraformaldehyde as formalin into, cost-saving, operation readiness.Preparation method of the present invention is simple, the production time is short, production efficiency is high, productive rate is high, production cost is lower.
Embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
A kind of based on safety reliable 9-Lumefantrine preparation method, the step of its preparation method is: (1), in reactor add ethyl formate, fluorenes, start stirring, is warming up to system temperature in 40-90 DEG C; (2), in batches add sodium methylate, heat release, and have bubble to produce, slowly add, finish, be warming up to backflow, temperature controls at 45-95 DEG C, insulation reaction, and TLC point plate tracks to and reacts completely; (3), lower the temperature, suction filtration, mother liquor adds formalin and stirs out solid, suction filtration, and solid is drained after adding washing, then uses high point petroleum ether recrystallization to obtain 9-Lumefantrine.
Claims (1)
1. based on a safety reliable 9-Lumefantrine preparation method, it is characterized in that: the step of this preparation method is:
(1), in reactor add ethyl formate, fluorenes, start stirring, be warming up to system temperature in 40-90 DEG C;
(2), in batches add sodium methylate, heat release, and have bubble to produce, slowly add, finish, be warming up to backflow, temperature controls at 45-95 DEG C, insulation reaction, and TLC point plate tracks to and reacts completely;
(3), lower the temperature, suction filtration, mother liquor adds formalin and stirs out solid, suction filtration, and solid is drained after adding washing, then uses high point petroleum ether recrystallization to obtain 9-Lumefantrine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310593957.7A CN104649866A (en) | 2013-11-21 | 2013-11-21 | Safe, reliable and low-cost preparation method of 9-fluorenylmethanol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310593957.7A CN104649866A (en) | 2013-11-21 | 2013-11-21 | Safe, reliable and low-cost preparation method of 9-fluorenylmethanol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104649866A true CN104649866A (en) | 2015-05-27 |
Family
ID=53241574
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310593957.7A Pending CN104649866A (en) | 2013-11-21 | 2013-11-21 | Safe, reliable and low-cost preparation method of 9-fluorenylmethanol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104649866A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112898130A (en) * | 2021-02-26 | 2021-06-04 | 太原理工大学 | Method for synthesizing 9-fluorenemethanol with high selectivity |
| CN113121316A (en) * | 2021-04-01 | 2021-07-16 | 孝义市金精化工有限公司 | Device and process for industrial synthesis of 9-fluorenylmethanol |
| WO2022141699A1 (en) * | 2020-12-29 | 2022-07-07 | 常州吉恩药业有限公司 | Method for preparing 9-fluorenyl formaldehyde |
-
2013
- 2013-11-21 CN CN201310593957.7A patent/CN104649866A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022141699A1 (en) * | 2020-12-29 | 2022-07-07 | 常州吉恩药业有限公司 | Method for preparing 9-fluorenyl formaldehyde |
| CN112898130A (en) * | 2021-02-26 | 2021-06-04 | 太原理工大学 | Method for synthesizing 9-fluorenemethanol with high selectivity |
| CN112898130B (en) * | 2021-02-26 | 2023-05-16 | 太原理工大学 | Method for synthesizing 9-fluorenylmethanol with high selectivity |
| CN113121316A (en) * | 2021-04-01 | 2021-07-16 | 孝义市金精化工有限公司 | Device and process for industrial synthesis of 9-fluorenylmethanol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101891649B (en) | Novel 3-cyano methyl benzoate preparing method | |
| CN109232578B (en) | Method for continuously preparing tetranitrobenzene pyridine tetraazapentalene (BPTAP) by using micro-reaction technology | |
| CN104649866A (en) | Safe, reliable and low-cost preparation method of 9-fluorenylmethanol | |
| CN102993246A (en) | Method for synthesizing isopropyl-beta-D-thiogalactoside | |
| CN105330568B (en) | Preparation method for p-aminobenzamidine hydrochloride | |
| CN102452902A (en) | Preparation method for phloroglucinol | |
| CN102924386A (en) | Industrial preparation method of 4-bromopyridazine | |
| CN103980097A (en) | Method for synthesizing phenols by etherifying | |
| CN103193608A (en) | Method for preparing dimethoxy benzaldehyde from veratrole | |
| CN102351790B (en) | Method for synthesizing 7-bromo-6-chloro-4-quinazolinone | |
| CN102731333B (en) | Method for preparing tetracaine | |
| CN104262109B (en) | A kind of synthetic method of resorcinol | |
| CN105175218A (en) | Preparation method of dichloro-p-xylene cyclic dimer | |
| CN103601715B (en) | A kind of separating and purifying method of 2-(4-fluorophenyl) thiophene | |
| CN100537552C (en) | Method for preparing Repaglinide | |
| CN103664835A (en) | Preparation method of biological plasticizing agent epoxidized fatty acid methyl ester | |
| CN103665063B (en) | A kind of method preparing isopropyl-β-D-thiogalactoside(IPTG) | |
| CN108129300A (en) | A kind of novel preparation method of acetylsalicylic acid | |
| CN104370830A (en) | Synthetic method of 5-trifluoromethyl uracil | |
| CN104557752A (en) | Synthetic method of 1,3,5-tris(4-tert-butyl-3-hydroxy-2,6-dimethylbenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione compound | |
| CN103387519B (en) | Preparation method for 4-hydroxybenzyl cyanide | |
| CN102086147B (en) | Preparation method of substituted phenol | |
| CN104447241A (en) | Process for separating methylal and methanol | |
| CN103694284B (en) | A kind of preparation technology of isopropyl-β-D-thiogalactoside(IPTG) | |
| CN103694285B (en) | A kind of preparation method of isopropyl-β-D-thiogalactoside(IPTG) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150527 |
|
| WD01 | Invention patent application deemed withdrawn after publication |