HRID1664499

反应详情

EQUATION

反应方程式

HRID 1664499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Crude ethyl (±)-(3-chlorocarbonyl-1,2,3,4-tetrahydro-carbazol-9-yl)-acetate (5 mmol) is dissolved in dry CH2Cl2 and treated with (R)-1-phenyl-ethanol (0.55 g, 5.4 mmol), DIEA (1.94 g, 15 mmol) and DMAP (61 mg, 0.5 mmol). The resulting yellow solution is stirred at rt overnight, diluted with EtOAc and successively washed with 0.1 N HCl, saturated aqueous NaHCO3, H2O and brine. The organic layer is dried over Na2SO4, filtered and evaporated. The residue is purified by column chromatography on silica gel (hexane/EtOAc 5:1) to provide the subtitle compound as yellow oil (1.36 g) in 76% yield.

WORKUP

后处理

  1. washsuccessively washed with 0.1 N HCl, saturated aqueous NaHCO3, H2O and brine
  2. dry with materialThe organic layer is dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. customThe residue is purified by column chromatography on silica gel (hexane/EtOAc 5:1)