Method for industrial production of tulobuterol

A technology of tulobuterol and oxidant, applied in the field of drug synthesis, can solve the problems of difficult removal of toxic impurities and high content of impurities, and achieve the effects of reduced production costs, low cost of raw materials, and simple steps
CN110172028AInactive Publication Date: 2019-08-27ANHUI HEALSTAR PHARM CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
ANHUI HEALSTAR PHARM CO LTD
Publication Date
2019-08-27
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a method for industrial production of tulobuterol. The method comprises the following steps of 1, preparation of an intermediate II, wherein chloroacetophenone and an oxidant containing DMSO are added into a reaction kettle in sequence, a reaction is carried out for 1-1.5 hours under the condition of heat preservation, stirring is conducted until the reaction is completelyfinished, and through quenching, extraction, washing and concentration, the intermediate II is prepared; 2, preparation of a crude tulobuterol product, wherein the intermediate II, tert-butylamine, analcohol solvent and sodium borohydride are added into the reaction kettle in sequence and stirred, the reaction temperature is controlled, stirring is conducted until the reaction is completely finished, after concentration, extraction, washing and drying with a drying agent, filtration is conducted, and a filtrate is concentrated and recrystallized to obtain the crude tulobuterol product I; 3, refining of the tulobuterol, wherein the crude tulobuterol product I, an organic solvent and activated carbon for refinement of injection are recrystallized to obtain the refined tulobuterol. The industrial production method is green in reaction and simple in step and causes little pollution to the environment, the purity of the product is up to 99.95% or above, and the tulobuterol contains few impurities.
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Description

technical field

[0001] The invention relates to the technical field of drug synthesis, in particular to a method for industrial production of tulobuterol. Background technique

[0002] Tulobuterol, whose chemical name is 1-(2-chlorophenyl)-2-tert-butylaminoethanol, is a selective β2 receptor agonist developed by Abbot Corporation of Japan. Asthma drugs were approved for marketing and were used to treat chronic obstructive pulmonary disease (COPD) in 1998. Currently, they are mostly used as patches to treat children with asthma.

[0003] The method for synthesizing tulobuterol in the prior art mainly contains following four kinds:

[0004] 1. Using o-chloroacetophenone as the starting material, it is prepared by bromination, amination and reduction at the alpha position of the carbonyl group, and has the following impurities:

[0005]

[0006] 2. Using 2-chloroacetophenone as the starting material, it is prepared by selenium dioxide oxidation, reduction, and amination, a...

Claims

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