- Synthetic method of deuterium-labeled D9-clenbuterol hydrochloride
-
The invention belongs to the field of food safety and standard substance synthesis, and discloses a synthetic method of deuterium-labeled D9-clenbuterol hydrochloride. According to the method, 4-amino-3,5-dichloroacetophenone is taken as a raw material and subjected to three-step reaction including bromination, D9 tert-butyl amination and reduction, and deuterium-labeled D9-clenbuterol hydrochloride is generated. The method is simple to operate, reaction conditions are mild (most reactions are performed at room temperature), reaction routes are reasonable, the process is advanced, the processing method is simple, and a product is easy to purify. Meanwhile, the total conversion rate of D9-tert-butylamine as the core raw material in the synthesis process of D9-clenbuterol hydrochloride is increased to 40% from 4.2%, yield is increased to 64%, and the method has good economic value and social value.
- -
-
Paragraph 0015; 0050-0051
(2019/01/14)
-
- Deuterium marked D9 Synthesis method of clenbuterol hydrochloride and synthesis method of synthetic intermediate thereof
-
The invention relates to a synthesis method of D9-clenbuterol hydrochloride labeled by deuterium as a stable isotope, in particular relates to a synthesis method of a synthesis intermediate of the D9-clenbuterol hydrochloride labeled by deuterium and belongs to the field of standard product synthesis and commodity inspection. According to the synthesis methods disclosed by the invention, 4-amino-alpha-bromine-3, 5-dichloroacetophenone reacts with D9-tert-butylamine, a feed ratio is changed, and other organic bases are selected to replace the D9-tert-butylamine to provide an alkali environment, so that the D9-tert-butylamine is only used for participating in reaction, and thus the conversion rate of the D9-tert-butylamine is remarkably increased. Compared with the prior art, the synthesis methods has the advantage that the use of expensive raw materials is reduced, the utilization ratio of D9-tert-butylamine is increased, a reduction method is optimized, the reduction yield is increased and reaches up to 94 percent, the chemical purity of products reaches 99 percent, and the products have good economical value.
- -
-
-