HRID1693134

反应详情

EQUATION

反应方程式

HRID 1693134 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 5-fluoro-3-methyl-indole (CAS: 392-13-2, 2.5 g) in DMF (20 ml) was added potassium hydroxide (1.41 g). The suspension was stirred at rt for 1 h and iodomethane (2.85 g) was added dropwise at 0-5° C. The reaction mixture was stirred at rt for 18 h and concentrated under high vacuum. The residue was quenched with water and extracted with ethyl acetate. The organics were washed, dried and concentrated. The crude residue was chromatographed on silica gel using heptane/ethyl acetate as eluent to obtain the desired compound (2.15 g) as a colorless liquid. MS (EI): 163.1 (M)

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at rt for 18 h
  2. concentrationconcentrated under high vacuum
  3. customThe residue was quenched with water
  4. extractionextracted with ethyl acetate
  5. washThe organics were washed
  6. customdried
  7. concentrationconcentrated
  8. customThe crude residue was chromatographed on silica gel