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Method for preparing propionyl bromine

A technology of propionyl bromide and propionic acid is applied in the field of preparation of propionyl bromide, can solve the problems of large equipment investment, high raw material cost, long production process time, etc., and achieves simple process operation, low raw material cost and stable product quality. Effect

Inactive Publication Date: 2010-06-30
上海三爱思试剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industry generally adopts the phosphorus tribromide method. The phosphorus tribromide method is the reaction of propionic acid and phosphorus tribromide. The solvent and the hydrobromic acid gas of the reaction are removed by distillation, and the propionyl bromide product is obtained through distillation. High cost of raw materials, long production process, large investment in equipment, low yield

Method used

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  • Method for preparing propionyl bromine

Examples

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Effect test

Embodiment 1

[0017] Example 1, 88.8 g of 1.2 mol propionic acid, 650 g of solvent 1,2-dichloropropane and 50 g of catalyst red phosphorus were added to the reaction vessel. Heat up to 90°C with stirring, drop 1.0 mol of bromine 80g, and reflux for 10 hours. After the reaction is completed, heat up to 94°C and collect 1,2-dichloropropane. After the end, heat up to 103°C-105°C. The propionyl bromide product was collected to obtain 89g of pure product with a yield of 65% and a content of 99.08%.

Embodiment 2

[0018] Example 2, add 96.2g of 1.3mol propionic acid, 720g of solvent 1,2-dichloropropane and 54g of catalyst red phosphorus into the reactor, heat up to 85°C under stirring, drop 88g of 1.0mol of bromine, and reflux for 12 Hours, the reaction is over, heat up to 94°C, collect 1,2-dichloropropane, after the end, heat up to 103°C to 105°C, collect the propionyl bromide product, and obtain the pure product 98.58, and the yield at 103°C to 105°C is 64.7%, the content is 98.96%.

Embodiment 3

[0019] Example 3, add 1.52mol of propionic acid 111g, solvent 1,2-dichloropropane 850g and catalyst red phosphorus 62g into the reactor, stir and raise the temperature to 90°C, add 1.3mol of bromine 104g dropwise, and reflux for 10 hours , when the reaction is over, heat up to 94°C to collect 1,2-dichloropropane. After the end, raise the temperature to 103°C to 105°C to collect the propionyl bromide product to obtain 117.5g of pure product, and the yield at 103°C to 105°C is 65.98 %, the content is 99.16%.

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Abstract

The invention discloses a method for preparing propionyl bromine. Propionic acid and bromine are used as raw materials; red phosphorus is used as catalyst; and low-level alkyl halide is used as solvent. The method comprises the following steps of: adding propionic acid, the solvent and the phosphorus catalyst into a reactor, stirring and rising temperature to between 80 and 90 DEG C, dropwise adding bromine, reflowing reacting for 10 to 12 hours, rising temperature to between 92 and 97 DEG C, collecting the solvent, rising temperature to between 103 and 105 DEG C, and then collecting pale yellow or transparent liquid, namely the propionyl bromine. The propionyl bromine is used as the special selective bromination base for nucleoside medicament. The content of the propionyl bromine is important to the medicament. The nucleoside medicament is a new type medicament used for curing AIDS and cancer.

Description

technical field [0001] The present invention relates to a kind of preparation method of propionyl bromide, relate to a kind of method of preparing propionyl bromide more precisely with propionic acid and bromine as raw material, red phosphorus as catalyst. Background technique [0002] Propionyl bromide is a light yellow or colorless transparent fuming liquid, miscible in acetonitrile and 1,2-dichloropropane, decomposed by alcohol when meeting water, with a density of 1.521 and a boiling point of 103-105°C. As a special selective bromination group of nucleoside drugs, its content is very important to the drug, and nucleoside drugs are new drugs used to treat AIDS and cancer patients. [0003] The conventional preparation method of propionyl bromide ("Fine Chemicals and Pharmaceutical Intermediates Handbook" P1~292) (e-ERDS Eneyolopedia of Reagents for OrganicSynthesis; Nopp given; 2001) (Synthesis (8) 684-7 1982, Synthesis (3 ) 216-18; 1981) is the reaction of phosphorus tr...

Claims

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Application Information

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IPC IPC(8): C07C53/42C07C51/60
Inventor 曾勇强
Owner 上海三爱思试剂有限公司