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Monoethyl oxalyl chloride and preparation method thereof

A technology for monoethyl oxalyl chloride and a production process, which is applied in the preparation of carboxylic acid halides, organic chemistry, etc., can solve the problems of difficult control of the production process, low product yield, and many by-products, and achieve good product quality and process The effect of simple route and less equipment

Active Publication Date: 2010-02-03
HAIMEN BEST FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Difficult to control in order to overcome existing monoethyl oxalyl chloride production technology, product yield is low, many by-products, the deficiency such as serious pollution, the invention provides a kind of monoethyl oxalyl chloride and production technology thereof, make its production technology simplify, Easy to control, high yield

Method used

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  • Monoethyl oxalyl chloride and preparation method thereof

Examples

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Embodiment 1

[0020] Embodiment 1, a kind of monoethyl oxalyl chloride and its production process, take oxalyl chloride and absolute ethanol as raw materials, put diethyl oxalate as a diluent into a reaction kettle, and make it synthesized at a temperature of 24°C-28°C Reaction, the feed ratio of oxalyl chloride and dehydrated alcohol is 2.18, diethyl oxalate is 3.6 times of dehydrated alcohol, and reaction generates product monoethyl oxalyl chloride yield 85%, product purity 99.2% and by-product dioxalate Ethyl ester and hydrochloric acid, the reaction is stable and easy to control.

Embodiment 2

[0021] Embodiment 2, a kind of monoethyl oxalyl chloride and its production process, the raw materials, diluent and by-products are the same as those in Example 1, the synthesis reaction temperature is 20°C-25°C, the molecular ratio of feed is 1.70, and diethyl oxalate is the diluent It is 4.8 times that of absolute ethanol, and the yield of monoethyl oxalyl chloride produced by the reaction is 85.1%, the purity is 99%, and the reaction is stable.

Embodiment 3

[0022] Embodiment 3, a kind of monoethyl oxalyl chloride and its production process, the raw materials, diluent and by-products are the same as in Example 1, the difference is that the reaction temperature is 15°C-19°C, the molecular feed ratio is 2.15, and the diluent is 3.9 times, The yield of the obtained product monoethyl oxalyl chloride is 87%, the purity is 99%, the reaction is stable and easy to control, and the effect is good.

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Abstract

The invention discloses an organic chemical synthesis product monoethyl oxalyl chloride C4O3H5Cl and a preparation method thereof. The preparation method of the invention is characterized in that themethod adopts oxalyl chloride and absolute ethanol as raw materials and diethyl oxalate as diluent to perform one-step synthesis reaction and two-step rectification at 10-28 DEG C to extract product monoethyl oxalyl chloride and by-product diethyl oxalate and chlorhydric acid; the optimal reaction temperature is 15-19 DEG C, the product yield is 85-88%, the product purity is not less than 99%, theoptimal feed molecular ratio of oxalyl chloride to absolute ethanol is 1:1.15-2.18 and the dosage of diethyl oxalate used as the diluent of the reaction is 3.5-4.8 times of that of absolute ethanol.The preparation method of the invention is used to produce monoethyl oxalyl chloride which is used as the raw material for synthesizing antibiotics, high effective herbicides and organic chlorides. The beneficial effects of the invention are that the production process is simple, the device investment is less, the reaction is stable and controllable, the yield and purity of the product are high and three wastes which are contaminants can not be discharged.

Description

technical field [0001] The invention relates to an organic chemical synthesis product monoethyl oxalyl chloride and a production process thereof. Background technique [0002] Monoethyl oxalyl chloride, the English name is Ethyl oxalyl chloride, the molecular formula is C 4 o 3 h 5 Cl, the molecular structure is Appearance: Colorless transparent liquid, volatile and deliquescent, with a boiling point of 135°C, used as a raw material for the synthesis of antibiotics, high-efficiency herbicides and organic chlorides. According to ChemListy 48 847-57 (1954) report, use diethyl oxalate and thionyl chloride as raw materials, react to generate monoethyl oxalyl chloride+sulfur dioxide and ethyl chloride, and the reaction principle is [0003] (CH 3 CH 2 o 2 c) 2 +SOCl 2 →ClOC-COOCH 2 CH 1 +SO 2 +CH 3 CH 2 Cl [0004] This reaction is difficult to control, the product yield is low, and there are many by-products. According to the report of CA97 192816C Ger728532, di...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/14
Inventor 杨鹤炉徐斌黄振兴
Owner HAIMEN BEST FINE CHEM
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