HRID1840622

反应详情

EQUATION

反应方程式

HRID 1840622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The preparation was carried out analogously to W. Duczek et al., Synthesis, 37-38 (1996). A solution of 4.04 g (40 mmol) of triethylamine in 10 mL of dichloromethane was added at 0° C. to a solution of 8.94 g (40 mmol) of L-leucine tert-butyl ester hydrochloride and 3.4 g (40 mmol) of cyanomethyl formate in 60 mL of dichloromethane. The reaction solution was allowed to warm to room temperature, stirred overnight at room temperature and then washed twice with saturated NaCl solution. The phases were separated and the organic phase was dried over magnesium sulfate. After filtration and removal of the solvent in vacuo, the residue obtained was distilled in vacuo. Yield: 7.5 g (87%). Boiling point: 118° C./2.7 Pa (0.02 torr).

WORKUP

后处理

  1. customDuczek et al., Synthesis, 37-38 (1996)
  2. washwashed twice with saturated NaCl solution
  3. customThe phases were separated
  4. dry with materialthe organic phase was dried over magnesium sulfate
  5. filtrationAfter filtration and removal of the solvent in vacuo
  6. customthe residue obtained
  7. distillationwas distilled in vacuo