HRID2105571

反应详情

EQUATION

反应方程式

HRID 2105571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Methyl-5-nitroindoline. To a round-bottomed flask equipped with magnetic stirring was added 5-nitroindoline (0.82, 5.0 mmol, Aldrich), iodomethane (0.71g, 5.0 mmol, Aldrich), sodium hydroxide (0.24, 6 mmol) and DMF (20 mL). The reaction mixture was stirred at 25° C. for 3 h, diluted with water (50 mL), extracted with EtOAc (3×40 mL) and the combined extracts were concentrated in vacuo. Purification by silica gel chromatography 97:3 hexane:EtOAc) provided the title product. MS (ESI, pos. ion) m/z: 179 (M+1).

WORKUP

后处理

  1. customTo a round-bottomed flask equipped
  2. stirringThe reaction mixture was stirred at 25° C. for 3 h
  3. extractionextracted with EtOAc (3×40 mL)
  4. concentrationthe combined extracts were concentrated in vacuo
  5. customPurification by silica gel chromatography 97:3 hexane