HRID2204303

反应详情

EQUATION

反应方程式

HRID 2204303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ra—Ni (EtOH) (230 mmol) was added to a solution of 3-chloro-1-methyl-5-nitro-1H-pyridin-2-one (Step E6) (136 mmol) in MeOH (400 mL) and the mixture was stirred at rt under a hydrogen atmosphere for 97 h. The reaction mixture was filtered over celite and concentrated. The product was purified by flash chromatography to afford the title compound as a black solid. ESI-MS: tR=0.33 min, [M+H]+ 159/161 (LC-MS 1); TLC: Rf=0.28 (9:1 CH2Cl2/MeOH).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered over celite and
  2. concentrationconcentrated
  3. customThe product was purified by flash chromatography