Verapamil hydrochloride synthesis
- Product Name:Verapamil hydrochloride
- CAS Number:23313-68-0
- Molecular formula:C27H39ClN2O4
- Molecular Weight:491.06
52-53-9
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Yield:23313-68-0 95%
Reaction Conditions:
with hydrogenchloride in water;ethyl acetate at 0 - 30; for 1 h;Solvent;Temperature;
Steps:
3; 10; 5 [0070] Example 10: Preparation of Verapamil hydrochloride (I)
Verapamil (I A, 204g) was charged in ethyl acetate (2040ml) and stirred for about lOmin to about 15min at about 20°C to about 30°C. Hydrochloric acid (12% w/w in ethylacetate, 165ml) was slowly added to the reaction mass, while maintaining the temperature at about 20°C to about 30°C. The reaction mass was stirred at about 20°C to about 25°C and further cooled to about 0°C to about 5°C, stirred for about lh and filtered. The solid was dried under vaccum at about 45°C to about 55°C to obtain verapamil hydrochloride (I, 194g). Percentage Yield:95%; HPLC purity: 99.57%; O-desmethyl verapamil: ND, single max impurity:0.11%.
References:
WO2021/245504,2021,A1 Location in patent:Paragraph 0063; 0070; 0065
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