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Synthetic method of medical intermediate

A synthesis method and a technology for intermediates, which are applied in the field of synthesis of pharmaceutical intermediates, can solve the problems of complex industrialization process, large cost of raw materials, and high production cost, and achieve the effects of mature synthesis process, low purchase price, and reduced input cost.

Active Publication Date: 2015-04-15
NANJING OCEAN PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to provide a brand-new 2-((4R,6S)-6-formaldehyde group- The preparation method of 2,2-dimethyl-1,3 dioxane-4-yl)-methyl acetate, the synthetic route is as follows:

Method used

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  • Synthetic method of medical intermediate
  • Synthetic method of medical intermediate
  • Synthetic method of medical intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] The synthesis of embodiment 1 D-3-Me

[0093] Add 252ml of THF, 45.2g of D-2-Me, and 124ml of methanol into a dry three-necked flask, protect it with nitrogen, and lower it to -80°C. The THF solution of diethylmethoxyborane was added dropwise, the drop was completed in 10 minutes, and the reaction was carried out at -75°C for 20 minutes. Add 14.4g KBH4 at one time, control the temperature at -75~-80°C, react for 4h to spot plate detection, and react overnight at room temperature for 10h. Add glacial acetic acid dropwise to adjust pH=6, and desolvate under reduced pressure. 79.5 g of oil was obtained.

Embodiment 2

[0094] The synthesis of embodiment 2 D-3-Na

[0095] Add 29 g of D-3, 5 g of sodium hydroxide, 60 ml of methanol, and 30 ml of water into a 250 ml three-necked flask, and heat the reaction system to 40°C. After monitoring until the disappearance of the raw materials, the system was concentrated to dryness to obtain 22.2 g of the target product with a yield of 92%.

Embodiment 3

[0096] The synthesis of embodiment 3 D-3-Me

[0097] Add 18g of D-3-Na into a 250ml three-necked flask, add 24g of methyl iodide, 100mL of acetone, and 2.6g of tetrabutylammonium bromide, and heat the reaction system to 70°C. Monitored until the raw materials disappeared, the system was concentrated to dryness, 100ml of ethyl acetate and 50ml of water solution were added, the organic layer was dried with anhydrous sodium sulfate, filtered, and the organic layer was concentrated to obtain 15g of the target product, with a yield of 88%.

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Abstract

The invention relates to the field of chemical synthesis, and particularly relates to a synthetic method of a medicament intermediate. The problems that raw material cost is high, an industrial process is complex and production cost of a product is relatively high in a conventional synthetic route of industrial production are solved. Provided is a brand-new preparation method of 2-((4R,6S)-6-formyl-2,2-dimethyl-1,3-dioxane-4-yl)-methyl acetate. The 2-((4R,6S)-6-formyl-2,2-dimethyl-1,3-dioxane-4-yl)-methyl acetate is synthesized by taking 6-chloro-5-hydroxy-3-carbonyl-methyl caproate as a starting material. The medicament intermediate not only is low in production cost, but also is simple in production process and easy for industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing a drug intermediate. [0002] Background technique [0003] 2-((4R,6S)-6-formaldehyde-2,2-dimethyl-1,3-dioxane-4-yl)-methyl acetate is an important drug synthesis intermediate, its synthesis The cost and the purity of the target product in the final product directly affect the cost of drug synthesis and the promotion of industrial production of the synthetic route. [0004] At present, the commonly used synthesis method is still the one published in 1995-97. [0005] One way is: [0006] ; [0007] This method not only has complicated process steps, but also requires ozone oxidation to break the double bond in step 6, so as to obtain the target product. The preparation cost is high, the effective conversion rate is low, and the purity of the obtained product is not high. At the same time, since the raw material structure is not easy to obtain, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/06C07C69/675C07C67/11
CPCC07C51/412C07C67/11C07D319/06C07C69/675C07C59/115
Inventor 陈本顺周长岳徐秋斌
Owner NANJING OCEAN PHARMA TECH