HRID976053

反应详情

EQUATION

反应方程式

HRID 976053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 0.69 g (3.0 mmol) of methyl α-methyl-D-tryptophan in 20 mL THF was added 0.8 g (3.0 mmol) of bis-(cyclohexylmethyl)acetyl chloride followed by 0.5 mL of Et3N and the suspension stirred at room temperature for 3 days. The mixture was diluted with EtOAc and washed with 1N citric acid, H2O, and saturated NaCl. Drying over MgSO4 and removal of the solvent under reduced pressure left 1.4 g of the crude product as a foam. Chromatography on silica gel, eluting with CHCl3 /EtOAc (95/5) gave 0.91 g (65% yield) of the product as a white foam. The structure was confirmed by NMR and mass spectroscopy.

WORKUP

后处理

  1. washwashed with 1N citric acid, H2O, and saturated NaCl
  2. dry with materialDrying over MgSO4 and removal of the solvent under reduced pressure
  3. waitleft 1.4 g of the crude product as a foam
  4. washChromatography on silica gel, eluting with CHCl3 /EtOAc (95/5)