HRID2194950

反应详情

EQUATION

反应方程式

HRID 2194950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of Intermediate 6 (30 mg) in N,N-dimethylacetamide (1 ml) was added with K4[Fe(CN)6].3H2O (6.6 mg, Ald), sodium carbonate (5.5 mg), and palladium acetate (1.1 mg, WAKO), and stirred at 120° C. for 5 hours. The reaction mixture was added with water (3 ml), and ethyl acetate (3 ml×2) for extraction, and then successively washed with saturated aqueous sodium hydrogencarbonate, saturated aqueous ammonium chloride, and saturated brine, the organic layer was dried, and then the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (Yamazen, n-hexane:ethyl acetate=3:1), and the solvent was evaporated under reduced pressure by using a rotary evaporator to obtain the title compound (yield: 10 mg).

WORKUP

后处理

  1. washsuccessively washed with saturated aqueous sodium hydrogencarbonate, saturated aqueous ammonium chloride, and saturated brine
  2. customthe organic layer was dried
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by column chromatography (Yamazen, n-hexane:ethyl acetate=3:1)
  5. customthe solvent was evaporated under reduced pressure
  6. customa rotary evaporator