HRID80176

反应详情

EQUATION

反应方程式

HRID 80176 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

K2CO3 (1.39 g, 10.08 mmol) was added to a stirred solution of 3-bromo-5-chloro-1H-indole (775 mg, 3.36 mmol) in DMF (7.5 mL) and the resulting mixture was stirred for 30 minutes. This was followed by the addition of methyl iodide (572.5 mg, 4.03 mmol) at 0-5° C. and the stirring was continued for a further 2 hours at room temperature. The reaction was monitored by TLC (10% ethylacetate in hexane). The reaction mixture was partitioned between ice water and DCM. The organic layer was concentrated to afford the crude product. Purification by column chromatography on silica gel (5% ethylacetate in hexane) afforded 530 mg of 3-Bromo-5-chloro-1-methyl-1H-indole (65% yield).

WORKUP

后处理

  1. waitthe stirring was continued for a further 2 hours at room temperature
  2. customThe reaction mixture was partitioned between ice water and DCM
  3. concentrationThe organic layer was concentrated
  4. customto afford the crude product
  5. customPurification by column chromatography on silica gel (5% ethylacetate in hexane)