HRID1037632

反应详情

EQUATION

反应方程式

HRID 1037632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe reaction mass was heated to 50-55° C. the reaction mixture
  2. temperaturewas maintained at 50-55° C. for 12.0 hrs
  3. customAfter reaction completion, it
  4. customwas quenched in a mixture of methanol (400 L) and water (800 L)
  5. customwas adjusted to 9-9.2 with aqueous ammonia at below 20° C
  6. extractionThe product was extracted with methylene dichloride
  7. concentrationconcentrated
  8. customto obtain the product which