HRID1689784

反应详情

EQUATION

反应方程式

HRID 1689784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

In dimethylformamide (5 mL), combine ethyl 5-bromo-1H-indole-2-carboxylate (1.00 g, 13.7 mmole), potassium carbonate (1.4 g, 10 mmole), and methyl iodide (280 μL, 4.50 mmole). Heat the mixture to 50° C. for 18 hours. Cool to room temperature and partition between EtOAc and water. Extract with EtOAc (3×), wash with brine (3×), dry (MgSO4) and concentrate to provide crude material. The crude material is purified on 120 g silica gel with 0 to 50% EtOAc in heptane to give 850 mg (81%) of the title compound. ES/MS m/e (81Br) 284.0 (M+H)+.

WORKUP

后处理

  1. temperatureCool to room temperature
  2. custompartition between EtOAc and water
  3. extractionExtract with EtOAc (3×)
  4. washwash with brine (3×)
  5. dry with materialdry (MgSO4)
  6. concentrationconcentrate
  7. customto provide crude material
  8. customThe crude material is purified on 120 g silica gel with 0 to 50% EtOAc in heptane