HRID379890

反应详情

EQUATION

反应方程式

HRID 379890 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 2-(4-acetoxymethyl-2-furoyl)-6-chloro-1-ethoxycarbonyl-3-(isovalerylamino)indole (step 3, 213.5 mg, 0.437 mmol) in ethanol (1.5 ml) was added 2N aqueous sodium hydroxide (1.5 ml). After stirring for 5.5 h, the mixture was poured into saturated aqueous ammonium chloride (20 ml) and extracted with ethyl acetate (80 ml). The organic layer was washed with brine (20 ml), dried (MgSO4) and cocentrated. The residue was purified by flash column chromatography eluting with ethyl acetate/hexane (1/3) and recrystallization from 2-propanol/isopropyl ether to give 119 mg (88%) of the titled compound as yellow solids. m.p: 200-201° C.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (80 ml)
  2. washThe organic layer was washed with brine (20 ml)
  3. dry with materialdried (MgSO4)
  4. customThe residue was purified by flash column chromatography
  5. washeluting with ethyl acetate/hexane (1/3) and recrystallization from 2-propanol/isopropyl ether