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Process for preparing cyclopropyl methyl ketone

A technology of cyclopropyl methyl ketone and pentanone, which is applied in the field of preparation of cyclopropyl methyl ketone, can solve the problems of difficult control of side reactions, low raw material utilization rate, large material consumption, etc., and achieve easy control of reactions, Effects of improving utilization rate and shortening production process

Active Publication Date: 2007-07-11
ANHUI JIXI COUNTY HUIHUANG CHEM
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AI Technical Summary

Problems solved by technology

But because it is a mixed reaction, the product is easy to enolize, and it is easy to generate polymer at high temperature, the side reaction is not easy to control, the utilization rate of raw materials is low, the material consumption is large, the reaction time is long, and the use of KOH is high in cost and low in yield. high

Method used

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  • Process for preparing cyclopropyl methyl ketone
  • Process for preparing cyclopropyl methyl ketone
  • Process for preparing cyclopropyl methyl ketone

Examples

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example 1

[0027] Example 1: Synthesis of 5-chloro-2-pentanone

[0028] Add 193g of 30% HCl (the amount of HCl is 1.5mol) into a 1000ml three-necked flask, stir and heat to 90°C, start to add 102g (1mol) of acetyl n-propanol dropwise, and complete the dropwise addition within one hour. Continue to keep the temperature for 2 hours, cool, separate the organic layer, and vacuum distill to obtain 105 g (yield: 87.4%) of a light yellow transparent liquid product, with a purity of 98.2% by GC analysis.

example 2

[0029] Example 2: Synthesis of Cyclopropyl Methyl Ketone

[0030] Add 120.6g (purity 98.2%, 1mol) of 5-chloro-2-pentanone to a solution composed of 70.6g soda lime and 50g water, heat to 65-75°C (preferably 70°C), and stir for 1 hour, Insulated for 2 hours, separated into layers, 90 g of the crude product in the organic layer was separated, 86 g was processed, and 72 g of pure product was obtained by distillation (yield 86.6%). The purity by GC analysis was 99.4%, and it was a colorless transparent liquid. Soda lime is composed of 5-10% NaOH and 90-95% CaO.

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Abstract

The invention discloses a making method of cyclopropyl methyl ketone, which comprises the following steps: adding normal aceto propyl alcohol in the alcaine solution; chlorinating; evaporating 5-chloride-2-pentanone; adopting separating coupling technique to do ringed-reaction for 5-chloride-2-pentanone; generating cyclopropyl methyl ketone.

Description

technical field [0001] The invention belongs to a preparation method of cyclopropyl methyl ketone. Background technique [0002] The production technology of cyclopropyl methyl ketone, existing technology mainly has three kinds of technical approaches: 1, adopt ethyl acetoacetate as raw material through three-step synthesis cyclopropyl methyl ketone, then it is prepared by oxidation with sodium hypohalite Cyclopropane carboxylic acid; 2. Use α-acetyl-γ-butyrolactone to generate 5-halogenated-2-pentanone by halogenation reaction in water medium at 10-30°C, and carry out 5-halogenated-2-pentanone The dehydrohalogenation cyclization reaction generates cyclopropyl methyl ketone; 3, from one or more carboxylic acids, with niobium and catalyst, the ketone is prepared under the condition of rising temperature, this process is beneficial to the preparation of cyclopropyl methyl ketone from cyclopropyl carboxylic acid and acetic acid Methyl ketones are particularly useful. 4. Using...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/11C07C45/61
Inventor 程捷程维兹胡小健程跃中刘辉来胡亦兵
Owner ANHUI JIXI COUNTY HUIHUANG CHEM
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