Unlock instant, AI-driven research and patent intelligence for your innovation.

Synthetic method of 1-chlorine-3-methoxy propane

A technology of methoxypropane and a synthesis method, which is applied in the field of preparation of 1-chloro-3-methoxypropane, can solve the problems of inability to meet large-scale industrial production, expensive imported reagents, and high production cost, and achieves low cost , easy operation, mild reaction conditions

Inactive Publication Date: 2009-08-12
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Some of the above methods have low yields; some need to use 1,3-propanediol raw material, which has not yet been produced in China. At present, only German Degussa Company, U.S. Shell Company and Dapont Company produce, but the imported reagents are expensive and the production cost is high. And it is difficult to obtain, which cannot meet the needs of domestic large-scale industrial production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthetic method of 1-chlorine-3-methoxy propane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The preparation of the benzene dispersion of embodiment 1 anhydrous sodium methylate

[0017] In a 500ml three-necked flask, add 300g (1.5mol) of methanol solution of 27% sodium methoxide, under magnetic stirring, recover the methanol under reduced pressure, pass in nitrogen protection, add 300ml of benzene to obtain the benzene dispersion of anhydrous sodium methoxide for later use, other The solvent dispersant is similar.

Embodiment 2

[0018] Example 2 Preparation of 1-chloro-3-methoxypropane

[0019] Add 300ml of sodium methoxide benzene dispersion into the dropping funnel with a balance tube, and add 236.2g (1.5mol) of 1,3-bromochloropropane in a 500ml four-necked flask equipped with a stirring blade, a thermometer, and nitrogen protection, and anhydrous Tetrabutylammonium bromide (TBAB) 6g, oil bath heating control external temperature 80 ℃, drop in 5 hours, heat preservation reaction 3 hours, sampling GC detects that reaction is finished completely, cools, and filters out inorganic salt sodium bromide, uses Wash with benzene, combine the filtrates, wash the benzene layer with water three times, measure the pH of the water = 6-7, near neutral, dry over anhydrous sodium sulfate, filter, and collect the 110°-112°C fraction of the filtrate to obtain the target product 1- 151 g of chloro-3-methoxypropane (92.8% yield).

Embodiment 3

[0020] Example 3 Preparation of 1-chloro-3-methoxypropane

[0021] Add 300ml of petroleum ether dispersion of anhydrous sodium methylate in the dropping funnel with balance tube, in the 500ml four-necked flask equipped with stirring blade, thermometer, and nitrogen protection, add 220g (1.4mol) of 1,3-bromochloropropane, Anhydrous benzyltrimethylammonium chloride (BTMAC) 5g, heated in an oil bath to control the external temperature 60°C, drop it within 2 hours, keep it warm for 2 hours, take a sample and GC to detect that the reaction is complete, cool, filter to remove inorganic salt bromine Sodium chloride, washed with benzene, combined filtrate, washed benzene layer with water three times, measured water pH = 6-7, near neutral, dried over anhydrous sodium sulfate, filtered, and the filtrate was rectified at atmospheric pressure to collect fractions at 110°-112°C to obtain 140 g of the target product 1-chloro-3-methoxypropane (92.2% yield).

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

A process for synthesizing 1-Cl-3-methoxy propane includes such steps as dripping the sodium methylate dispersed in inertial solvent into 1,3-bromochloropropane under existence of phase-transfer catalyst, reacting, filtering for removing sodium bromide, washing the filtered cake by inertial solvent, collecting organic layer, water washing until pH=5-7 to obtain coarse product, drying, filtering, and rectifying filtrate.

Description

technical field [0001] The invention belongs to the field of organic chemistry, in particular to a preparation method of 1-chloro-3-methoxypropane. Background technique [0002] 1-Chloro-3-methoxypropane is an important intermediate of organic compounds and has a wide range of uses. It has been studied as early as the beginning of last century, such as (CA3:1173) Acad Sci Fennicae 3A, 1-103 and (CA27:1615 3 )Org.Synthesis 8,112, Ann Chim 18 303-94,1932, with 1,3-propanediol to prepare Cl(CH 3 ) 3 OH, followed by methylation with dimethyl sulfate to prepare 1-chloro-3-methoxypropane with a methylation yield of only 65%. [0003] (CA25:3958) from HO(CH 3 ) 3 Starting from OMe, 1-chloro-3-methoxypropane was obtained by halogenating phosphorus trihalide, and the yield was only 58~76%; (CA32:4141 8 ) BER.71B, 574-5 (1938) prepared in 90% yield from 1,3-propanediol. [0004] (CA46:1443 1 ) J.OOrg Chem 16, 704-7 (1951) and (CA52:17320 e ) Compt rend246, 1868-7 etc. from HO ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/01C07C43/12
Inventor 陈建辉叶伟东王燕
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY