HRID926360

反应详情

EQUATION

反应方程式

HRID 926360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 6-((S)-2-methyl-pyrrolidine-1-carbonyl)-3,4-dihydro-1H-pyrrolo[2,1-c][1,4]oxazine-8-carboxylic acid ethyl ester (Comp. No. 6c) (762 mg, 2.49 mmol) in methanol (10 ml) was added water (4 ml) and 2 N aqueous potassium hydroxide (6 ml, 12 mmol). The mixture was stirred for 3 h at 80° C., then cooled down to 25° C. and acidified with excess 10 M aqueous hydrochloric acid. After extraction (3 times with dichloromethane), the combined organic layers were dried over sodium sulfate and the solvents evaporated to give 595 mg (86%) 6-((S)-2-methyl-pyrrolidine-1-carbonyl)-3,4-dihydro-1H-pyrrolo[2,1-c][1,4]oxazine-8-carboxylic acid as a white solid. LC/MS (method 2): Rt=0.98 min; m/z=279.06 (M+H+).

WORKUP

后处理

  1. temperaturecooled down to 25° C.
  2. extractionAfter extraction (3 times with dichloromethane)
  3. dry with materialthe combined organic layers were dried over sodium sulfate
  4. customthe solvents evaporated