HRID379913
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To a solution of 7-chloro-2-[(N-methoxy-N-methylamino)carbonyl]-3-nitroindole (step 2, 420 mg, 1.5 mmol) in ethanol-water (2:1, 30 ml) was added iron powder (168 mg, 3 mmol) and ammonium chloride (160 mg, 3 mmol). The mixture was heated at 50° C. for 2 h, and then cooled to room temperature. After filtration through a pad of Celite, the filtrate was concentrated. The residue was purified by flash column chromatography eluting with ethyl acetate/hexane (1:10˜1:1) to give 287 mg (75%) of the title compound.
WORKUP
后处理
- temperaturecooled to room temperature
- filtrationAfter filtration through a pad of Celite
- concentrationthe filtrate was concentrated
- customThe residue was purified by flash column chromatography
- washeluting with ethyl acetate/hexane (1:10˜1:1)