反应 #2171055

反应方程式

4-(5chloroindol-3-yl)-2-hydroxy-4-oxo-2-butenoic acid ethyl ester

methylamine acetate

→

titled compound

收率 38.0%

4-(5-Chloroindol-3-yl)-2-methylamino-4-oxo-2-butenoic acid ethyl ester

收率 38.0%

溶剂

EtOH

反应条件

后处理

1. 1
   温度After refluxing for 2.5 hours
2. 2
   浓缩the reaction mixture was concentrated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
4. 4
   洗涤The ethyl acetate was washed with water
5. 5
   其他dried
6. 6
   浓缩concentrated
7. 7
   其他The resulting residue was chromatographed on silica gel (ethyl acetate as eluant)

实验过程

To a solution of 0.59 g (2.0 mmol) of 4-(5chloroindol-3-yl)-2-hydroxy-4-oxo-2-butenoic acid ethyl ester prepared in Example 1(1) in 95% EtOH (10 ml) was added 0.55 g (6.0 mmol) of methylamine acetate. After refluxing for 2.5 hours, the reaction mixture was concentrated and the residue was dissolved in ethyl acetate. The ethyl acetate was washed with water, dried, and then concentrated. The resulting residue was chromatographed on silica gel (ethyl acetate as eluant) to give 0.23 g of the titled compound as oil. Yield: 38%.

来源