HRID464900

反应详情

EQUATION

反应方程式

HRID 464900 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 1.00 g (3.8 mmole) of (2S,3S)-3-(t-butoxycarbonyl)amino-2-hydroxy-5-methylhexaneoic acid prepared according to the method of R. L. Johnson [J. Med. Chem., 25, 605 (1982)] in 30 ml. of methanol was added, with stirring and ice-cooling, an ethereal solution of diazomethane. The mixture was stirred at room temperature for 1 hour. The solvent was removed by distillation, and the solid thus obtained was recrystallized from hexane, to afford 952 mg. of colourless needles, melting at 84°-85° C.; [α]22 -10.2° (C=1.26, methanol).

WORKUP

后处理

  1. temperatureice-cooling
  2. stirringThe mixture was stirred at room temperature for 1 hour
  3. customThe solvent was removed by distillation
  4. customthe solid thus obtained
  5. customwas recrystallized from hexane
  6. customto afford 952 mg