HRID1618536

反应详情

EQUATION

反应方程式

HRID 1618536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred solution of methyl 2-methyl-2-(5-morpholino-3-nitropyridin-2-yl)-propanoate (1.2 g, 3.88 mmol) in acetic acid (22.2 mL, 388 mmol) was added iron powder (1.08 g, 19.40 mmol). The reaction was heated at 80° C. for 2 h. After this time the reaction was cooled to rt and filtered over Celite™. The Celite™ was washed with acetic acid and the combined filtrates were evaporated in vacuo. Purification by column chromatography (hexane:EtOAc, 1:0 to 0:1) gave 3,3-dimethyl-6-morpholino-1H-pyrrolo[3,2-b]pyridin-2(3H)-one. Mass Spectrum (ESI) m/e=248 (M+1).

WORKUP

后处理

  1. temperatureAfter this time the reaction was cooled to rt
  2. filtrationfiltered over Celite™
  3. washThe Celite™ was washed with acetic acid
  4. customthe combined filtrates were evaporated in vacuo
  5. customPurification by column chromatography (hexane:EtOAc, 1:0 to 0:1)