HRID324599

反应详情

EQUATION

反应方程式

HRID 324599 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 10.75 g (38.56 mmol) of trityl chloride is added, at 0° C., to a solution of 6 g (38.56 mmol) of L-serine methyl ester hydrochloride and 7.8 g (77.12 mmol) of triethylamine in absolute THF and this solution is left to stir at 0° C. for 4 h and then at room temperature for 2 days. The solvent is removed in vacuo and the residue is partitioned between dichloromethane and a 10% aqueous solution of citric acid. The phases are separated and the organic phase is washed with water and dried over sodium sulfate. Following filtration, the solvent is removed in vacuo and the residue is chromatographed through silica gel using heptane/ethyl acetate=6/4. 8 g (58%) of (34.3) are obtained after concentrating the product fractions.

WORKUP

后处理

  1. waitthis solution is left
  2. waitat room temperature for 2 days
  3. customThe solvent is removed in vacuo
  4. customthe residue is partitioned between dichloromethane
  5. customThe phases are separated
  6. washthe organic phase is washed with water
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltration
  9. customthe solvent is removed in vacuo
  10. customthe residue is chromatographed through silica gel