HRID1642529

反应详情

EQUATION

反应方程式

HRID 1642529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Acetyl-4-bromo-1H-indole-3-carbaldehyde (3.5 g, 13.2 mmol) was dissolved in CH2Cl2 (50 mL). 3-Chloroperbenzoic acid (3.9 g, 15.8 mmol) was added, and the reaction stirred 16 h at r.t. The solution was washed with sat. NaHCO3 and brine, dried (MgSO4), and concentrated. The residue was stirred with K2CO3 (100 mg) in MeOH (50 mL) for 2 min. The solution was concentrated and purified by silica gel chromatography (100% CH2Cl2) to give 880 mg (26%) of the title compound as a faintly blue solid. MS (ES) [m+H] calc'd for C10H8BrNO2, 254, 256; found 254, 256.

WORKUP

后处理

  1. washThe solution was washed with sat. NaHCO3 and brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. stirringThe residue was stirred with K2CO3 (100 mg) in MeOH (50 mL) for 2 min
  5. concentrationThe solution was concentrated
  6. custompurified by silica gel chromatography (100% CH2Cl2)