HRID1696759

反应详情

EQUATION

反应方程式

HRID 1696759 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 1-methyl-1-H-indol-7-ol (Chemstep, CAS: 47577-33-4, 2.2 g, 15 mmol) and 2-chloro-N,N-dimethylacetamide (Fluka, CAS: 2675-89-0, 2.0 g, 17 mmol) in acetone (25 mL) were added potassium carbonate (2.5 g, 18 mmol) and potassium iodide, (0.25 g, 1.5 mmol). The reaction mixture was stirred at reflux for 4 h, quenched with ice/water, and extracted with ethyl acetate. The organics were washed, dried and concentrated. The residue was chromatographed on silica gel using heptane/ethyl acetate as eluent to obtain the desired compound (2.9 g) as a creamy solid. MS (ISP): m/e 233.1 (M+H)+

WORKUP

后处理

  1. temperatureat reflux for 4 h
  2. customquenched with ice/water
  3. extractionextracted with ethyl acetate
  4. washThe organics were washed
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was chromatographed on silica gel