HRID1275785

反应详情

EQUATION

反应方程式

HRID 1275785 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.032 g (0.085 mmol) N-methyl--O--(9-phenyl-9H-fluoren-9-yl)-L-serine methyl ester from Step 1 in methanol (1 mL) was added 20% sodium hydroxide (1 mL) and the mixture stirred at room temperature for 1 h. Most of the ethanol was evaporated under vacuo, the residue suspended in water (5 mL) nd extracted with diethyl ether (2×1 mL). The alkaline aqueous phase was acidified with 20% acetic acid by cooling with an ice bath, the white precipitate was filtered, washed with water and dried in vacuo over P2O5 to give 0.027 g (yield 90%) N-methyl--O--(9-phenyl-9H-fluoren-9-yl)-L-serine as a white powder.

WORKUP

后处理

  1. customMost of the ethanol was evaporated under vacuo
  2. extractionextracted with diethyl ether (2×1 mL)
  3. temperatureby cooling with an ice bath
  4. filtrationthe white precipitate was filtered
  5. washwashed with water
  6. dry with materialdried in vacuo over P2O5