HRID1037632
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 17.5 °C
PROCEDURE
实验过程
30 kg of DL-Methionine was added to a solution of methane sulphonic acid (390 kg) maintained at 15-20° C. and stirred for 30 minutes. To this solution, 4,5α-Epoxy-14-hydroxy-3-methoxy-17-methylmorphinan-6-one (40 kg) was added at 20° C. and the reaction mass was heated to 50-55° C. the reaction mixture was maintained at 50-55° C. for 12.0 hrs. After reaction completion, it was quenched in a mixture of methanol (400 L) and water (800 L) and the pH of the resultant solution was adjusted to 9-9.2 with aqueous ammonia at below 20° C. The product was extracted with methylene dichloride and concentrated to obtain the product which was isolated with cyclohexane. Yield: 33.4 kg
WORKUP
后处理
- temperaturethe reaction mass was heated to 50-55° C. the reaction mixture
- temperaturewas maintained at 50-55° C. for 12.0 hrs
- customAfter reaction completion, it
- customwas quenched in a mixture of methanol (400 L) and water (800 L)
- customwas adjusted to 9-9.2 with aqueous ammonia at below 20° C
- extractionThe product was extracted with methylene dichloride
- concentrationconcentrated
- customto obtain the product which