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Preparation method of ethyl 4-chloroacetoacetate

A technology of ethyl chloroacetoacetate and ethyl acetoacetate is applied in the field of preparation of ethyl 4-chloroacetoacetate, and can solve the problems such as low efficiency of ethyl 4-chloroacetoacetate, inability to meet the requirements of the preparation method, and the like, Accurate and stable temperature control, easy to implement, and simple steps

Active Publication Date: 2020-11-20
JIANGSU HENGAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Ethyl 4-chloroacetoacetate is often used as an intermediate for medicine and pesticides. The efficiency of traditional synthetic preparation methods for preparing ethyl 4-chloroacetoacetate is too low. Now ethyl acetoacetate and sulfuryl are used as raw materials to quickly prepare The crude product of ethyl 4-chloroacetoacetate, and the present synthetic equipment structure cannot meet the requirements of the above-mentioned preparation method

Method used

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  • Preparation method of ethyl 4-chloroacetoacetate
  • Preparation method of ethyl 4-chloroacetoacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method for ethyl 4-chloroacetoacetate, comprising the steps of:

[0027] Step 1: First, add ethyl acetoacetate in the reactor, and cool it to 05°C;

[0028] Step 2: Then add sulfuryl chloride dropwise to the reactor, keeping the temperature of the reaction solution at 0°C;

[0029] Step 3: After the dropwise addition, stir and react at room temperature for 2 hours;

[0030] Step 4: Then remove the gas in the reactor under the condition of 35°C;

[0031] Step 5: Then, the unreacted ethyl acetoacetate is recovered by distillation when the temperature is raised to 85°C;

[0032] Step 6: Finally, cool to 30°C to obtain crude ethyl 4-chloroacetoacetate.

[0033] The molar ratio of ethyl acetoacetate and sulfuryl chloride is 4.5:4.

Embodiment 2

[0035] A preparation method for ethyl 4-chloroacetoacetate, comprising the steps of:

[0036] Step 1: First, add ethyl acetoacetate in the reactor, and cool it down to 2.5°C;

[0037] Step 2: Then add sulfuryl chloride dropwise to the reactor, keeping the temperature of the reaction solution at 2.5°C;

[0038] Step 3: after the dropwise addition, stir and react at room temperature for 3 hours;

[0039] Step 4: then remove the gas in the reactor under the condition of 45°C;

[0040] Step 5: Then, the unreacted ethyl acetoacetate is recovered by distillation when the temperature is raised to 90°C;

[0041] Step 6: Finally, cool to 30°C to obtain crude ethyl 4-chloroacetoacetate.

[0042] The molar ratio of ethyl acetoacetate and sulfuryl chloride is 5.05:4.5.

Embodiment 3

[0044] A preparation method for ethyl 4-chloroacetoacetate, comprising the steps of:

[0045] Step 1: First, add ethyl acetoacetate in the reactor, and cool it to 5°C;

[0046] Step 2: Then add sulfuryl chloride dropwise to the reactor, keeping the temperature of the reaction solution at 5°C;

[0047] Step 3: after the dropwise addition, stir and react at room temperature for 4 hours;

[0048] Step 4: Then, the gas in the reactor is pumped out under the condition of 55° C.;

[0049] Step 5: Then, the unreacted ethyl acetoacetate is recovered by distillation when the temperature is raised to 95°C;

[0050] Step 6: Finally, cool to 30°C to obtain crude ethyl 4-chloroacetoacetate.

[0051] The molar ratio of ethyl acetoacetate and sulfuryl chloride is 5.6:5.

[0052] The reactor in the preparation method of ethyl 4-chloroacetoacetate proposed by the present invention can realize the rapid production of crude ethyl 4-chloroacetoacetate by using ethyl acetoacetate and sulfuryl ...

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Abstract

The invention discloses a preparation method of ethyl 4-chloroacetoacetate. The preparation method comprises the following steps: step one, adding ethyl acetoacetate into a reactor, and cooling to 0-5DEG C; step two, dropwise adding sulfuryl chloride into the reactor, and keeping the temperature of the reaction solution at 0-5 DEG C; step three, after dropwise adding is completed, reacting for 2-4 hours under stirring at the room temperature; step four, pumping out the gas in the reactor at a temperature of 35-55 DEG C; step five, heating to 85-95 DEG C, and distilling and recovering the unreacted ethyl acetoacetate; and step six, finally cooling to 30 DEG C to obtain a crude product of ethyl 4-chloroacetoacetate. The method is simple in steps and convenient to implement, can realize rapid preparation of the crude product of ethyl 4-chloroacetoacetate by taking ethyl acetoacetate and sulfuryl chloride as raw materials, is high in preparation speed, and can realize recovery of unreacted ethyl acetoacetate.

Description

technical field [0001] The invention relates to the field of chemical preparation, in particular to a preparation method of ethyl 4-chloroacetoacetate. Background technique [0002] Ethyl 4-chloroacetoacetate is often used as an intermediate for medicine and pesticides. The efficiency of traditional synthetic preparation methods for preparing ethyl 4-chloroacetoacetate is too low. Now ethyl acetoacetate and sulfuryl are used as raw materials to quickly prepare The crude product of ethyl 4-chloroacetoacetate, and the present synthetic equipment structure can not meet the requirements of the above-mentioned preparation method. Contents of the invention [0003] For solving the problems of the technologies described above, the invention provides a kind of preparation method of ethyl 4-chloroacetoacetate, comprising the steps: [0004] Step 1: First, add ethyl acetoacetate into the reactor, and cool it down to 0-5°C; [0005] Step 2: Then add sulfuryl chloride dropwise to th...

Claims

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Application Information

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IPC IPC(8): C07C69/72C07C67/307
CPCC07C67/307C07C69/72
Inventor 陈敏方
Owner JIANGSU HENGAN CHEM
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