HRID906474

反应详情

EQUATION

反应方程式

HRID 906474 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
67 °C

PROCEDURE

实验过程

(3R)-tert-Butyl 4-((6-(5-(cyclopropylcarbamoyl)-3-fluoro-2-methylphenyl)-2-(2,2-dimethyl-3-(pivaloyloxy)propyl)-1-oxo-1,2-dihydroisoquinolin-4-yl)methyl)-3-methylpiperazine-1-carboxylate (50.8 g) was dissolved in methanol (600 mL) and a solution of potassium carbonate (29.3 g) in water (100 mL) was added. The reaction was heated at reflux (internal temperature 67° C.) for 16 h. After cooling to 50° C., further water was slowly added until the mixture became opaque and the mixture was cooled to 23° C. over 1 h. The precipitate was collected by filtration, washed with water (100 mL) and isohexane (100 mL) and dried in vacuo at 45° C. to give the subtitle product (32.4 g).

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureAfter cooling to 50° C.
  3. temperaturethe mixture was cooled to 23° C. over 1 h
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water (100 mL) and isohexane (100 mL)
  6. customdried in vacuo at 45° C.