Preparation method of 2-acetoxyl group methoxy group-1.3-propylene dichloride
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A technology of acetoxymethoxy and dichloropropane, which is applied in the field of preparation of 2-acetoxymethoxy-1.3-dichloropropane, can solve the problems of high cost, inconvenient use, easy discoloration, etc. The effect of short time, less side reactions and less impurities
Inactive Publication Date: 2013-06-05
HUBEI BAOLE PHARMA
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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 still, collect 115°C / 10mmHg fractions to obtain 2-acetoxymethoxy-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 fractions 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, heat up 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 fractions, and obtain a weight yield of 90% and a content of ≥95%. 2-Acetoxymethoxy-1,3-dichloropropane.
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Abstract
Disclosed is a preparation method of 2-acetoxyl group methoxy group-1.3-propylene dichloride. The following substances are extracted according to weight ratio: 250kg of 1.3-dichloro-2-propyl alcohol, 60kg of paraformaldehyde, 3.68kg of vitriol, 250kg of acetic anhydride and 5kg of potassium acetate; the 1.3-dichloro-2-propyl alcohol, the paraformaldehyde and the vitriol are added to a clean and dry reaction still and are warmed slowly, the temperature rises to 96 DEG C to 98 DEG C in 2 hours, and heat preservation is carried out for 2 hours; the temperature is lowered to 10 DEG C after heat preservation, the acetic anhydride is dropped to the reaction still, and the temperature is kept between 15 DEG C and 20 DEG C; after the acetic anhydride is added, the temperature rises to 35 DEG C to 40 DEG C, and heat preservation is carried out for 10 hours; the potassium acetate is added to the reaction still, stirring is conducted, the acetic anhydride is recycled in vacuum to 100 DEG C, the temperature is lowered to 20 DEG C, and filtering is conducted; and filter liquor is pumped into a rectifying still, steamed cut fraction in a state of 115 DEG C/10mmHg is collected, and the 2-acetoxyl group methoxy group-1.3-propylene dichloride with 80% of weight yield and more than or equal to 95% of content is obtained. According to the preparation method of the 2-acetoxyl group methoxy group-1.3-propylene dichloride, production cost is reduced, and yield is improved.
Description
technical field [0001] The invention belongs to the field of chemical industry or pharmacy, and specifically refers to a preparation method of 2-acetoxymethoxy-1.3-dichloropropane. Background technique [0002] 2-Acetoxymethoxy-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 concentrat...
Claims
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