Preparation method of 2-acetylchloromethoxy-1,3-dichloropropane

A technology of chloromethoxy and dichloropropane, which is applied in the field of preparation of 2-acetylchloromethoxy-1.3-dichloropropane, can solve the problems of high cost, inconvenient use, easy discoloration and the like, and achieves the reaction time Short, less side reactions, the effect of quality improvement

Inactive Publication Date: 2013-03-06
HUBEI BAOLE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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  • Preparation method of 2-acetylchloromethoxy-1,3-dichloropropane
  • Preparation method of 2-acetylchloromethoxy-1,3-dichloropropane
  • Preparation method of 2-acetylchloromethoxy-1,3-dichloropropane

Examples

Experimental program
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Embodiment 1

[0030] Extract the following substances by weight ratio:

[0031]

[0032] In a clean and dry reaction kettle, add 1.3-dichloro-2-propanol, paraformaldehyde, and sulfuric acid, slowly raise the temperature, raise the temperature to 96-98°C in 2 hours, keep it warm for 2 hours, after the heat preservation is completed, cool down to 10°C and start dripping Add acetic anhydride, keep the temperature at 15-20°C, after the addition, raise the temperature at 35-40°C and keep it warm for 10 hours, add potassium acetate, stir, recover the acetic anhydride in vacuum to 100°C, cool down to 20°C, filter, and pump the filtrate into the refined In the distillation still, collect 115°C / 10mmHg distillate to obtain 2-acetylchloromethoxy-1.3-dichloropropane with a weight yield of 80% and a content of ≥95%.

Embodiment 2

[0034] Starting from the second charge, extract the following substances by weight ratio:

[0035]

[0036]

[0037] In a clean and dry reaction kettle, add 1.3-dichloro-2-propanol, paraformaldehyde, sulfuric acid, slowly raise the temperature, raise the temperature to 96-98°C in 2 hours, keep it warm for 2 hours, after the heat preservation is complete, cool it down to 10°C, add 250kg of the distillate steamed below 115°C / 10mmHg during the rectification described in Example 1, then start to add acetic anhydride dropwise, the temperature remains at 15-20°C, after the addition is completed, the temperature is raised at 35-40°C for 10 hours, Add potassium acetate, stir, vacuum recover acetic anhydride to 100°C, cool down to 20°C, filter, pump the filtrate into a rectification kettle, collect 115°C / 10mmHg distillate to obtain 90% weight yield, content ≥ 95% 2-Acetylchloromethoxy-1,3-dichloropropane.

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Abstract

The invention relates to a preparation method of 2-acetylchloromethoxy-1,3-dichloropropane, which comprises the following steps: extracting the following substances: 250kg of 1,3-dichloro-2-propanol, 60kg of polyformaldehyde, 3.68kg of sulfuric acid, 250kg of acetic anhydride and 5kg of postassium acetate; adding the 1,3-dichloro-2-propanol, polyformaldehyde and sulfuric acid into a clean and dry reaction kettle, slowly heating to 96-98 DEG C within 2 hours, and keeping the temperature for 2 hours; after finishing keeping the temperature, cooling to 10 DEG C, and dropwisely adding the acetic anhydride while keeping the temperature at 15-20 DEG C; and after finishing the dropwise addition, heating to 35-40 DEG C, keeping the temperature for 10 hours, adding postassium acetate, stirring, recovering the acetic anhydride in vacuum to 100 DEG C, cooling to 20 DEG C, filtering, sucking the filtrate into a rectifying still, and collecting the fraction in the 115 DEG C/10mmHg state, thereby obtaining the 2-acetylchloromethoxy-1,3-dichloropropane of which the weight yield is 80% and the content is greater than or equal to 95%. The invention lowers the production cost and enhances the yield.

Description

technical field [0001] The invention belongs to the field of chemical industry or pharmacy, and specifically refers to a preparation method of 2-acetylchloromethoxy-1.3-dichloropropane. Background technique [0002] 2-Acetyl chloromethoxy-1.3-dichloropropane (hereinafter referred to as chloromethoxy ester) is the main intermediate of the antiviral raw material drug ganciclovir, and has a large market both domestically and internationally. Since the product was put into the domestic market in 1998, it has been using the initial process. Its characteristics are: 1. The production time is long, about five days (120h); 2. There are 5 steps in the production process; 3. Use a class of solvent pure benzene; 4. , Yield rate is only about 55%. [0003] Its chemical reaction equation is: [0004] first step: [0005] [0006] Step two: [0007] [0008] Operation: Add the prepared 1.3-dichloro-2-propanol into a clean and dry 1000L reactor and stir, add paraformaldehyde, add...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/24
Inventor 杨保廷
Owner HUBEI BAOLE PHARMA
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