HRID1637827

反应详情

EQUATION

反应方程式

HRID 1637827 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of (S)-(-)-4-[4-[5-[(acetylamino)methyl]-2-oxo-3-oxazolidinyl]-2-fluorophenyl]-1-piperidinecarboxylic acid phenylmethyl ester (EXAMPLE 20, Step 9, 10.44 g) in dry methylene chloride (100 mL) at 0° C. under N2 is treated with trifluoroacetic acid (24.0 mL) over one minute, and the resulting mixture is stirred at 0° C. for 1.75 hours, concentrated under reduced pressure, diluted with water (100 mL), cooled in an ice bath, adjusted to pH 11 with saturated aqueous potassium carbonate, and extracted with methanol/methylene chloride (5/95, 6×100 mL). The combined organic phase is dried over anhydrous sodium sulfate and concentrated under reduced pressure to give the title compound, mp 163-164° C.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. additiondiluted with water (100 mL)
  3. temperaturecooled in an ice bath
  4. extractionextracted with methanol/methylene chloride (5/95, 6×100 mL)
  5. dry with materialThe combined organic phase is dried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure