反应 #2171058

反应方程式

( 1 )

4-[1-(N,N-dimethylcarbamoyl)-5-chloroindol-3-yl]-2-hydroxy-4-oxo-2-butenoic acid diphenylmethyl ester

trifluoroacetic acid

→

titled compound

收率 67.0%

4-[1-(N,N-dimethylcarbamoyl)-5-chloroindol-3-yl]-2-hydroxy-4-oxo-2-butenoic acid

收率 67.0%

溶剂

dichloromethane

反应条件

后处理

1. 1
   workup.ADDITIONwas added under ice-
2. 2
   温度cooling
3. 3
   温度cooling
4. 4
   浓缩The reaction solution was concentrated under reduced pressure
5. 5
   workup.DISSOLUTIONThe residues was dissolved in ethyl acetate
6. 6
   洗涤The ethyl acetate was washed successively with water and brine
7. 7
   其他dried
8. 8
   其他The obtained residue was crystallized from ether
9. 9
   其他recrystallized from 95% ethanol

实验过程

To a solution of 356 mg (0.7 mmol) of the ester derivative obtained in above (1) in dichloromethane (3.6 ml) was added under ice-cooling, 0.5 ml of trifluoroacetic acid. The mixture was stirred for 30 minutes under ice-cooling. The reaction solution was concentrated under reduced pressure. The residues was dissolved in ethyl acetate. The ethyl acetate was washed successively with water and brine, and then dried. The obtained residue was crystallized from ether and recrystallized from 95% ethanol to give 0.16 g of the titled compound. Yield: 67%.

来源