反应 #2171056

ord-4edbe845fd6c43a0b187d98e0723ed2c

反应方程式

Cl
hydrochloric acid
CCOC(=O)C(=CC(=O)c1c[nH]c2ccc(Cl)cc12)NC
( 1 )
CCOC(=O)C(=CC(=O)c1c[nH]c2ccc(Cl)cc12)NC
4-(5-Chloroindol-3-yl)-2-methylamino-4-oxo-2-butenoic acid ethyl ester
[Na+].[OH-]
NaOH
CNC(=CC(=O)c1c[nH]c2ccc(Cl)cc12)C(=O)O
titled compound
收率 80.0%
CNC(=CC(=O)c1c[nH]c2ccc(Cl)cc12)C(=O)O
4-(5-Chloroindol-3-yl)-2-methylamino-4oxo-2-butenoic acid
收率 80.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩concentrated under reduced pressure
  2. 2
    workup.ADDITIONThe residue was diluted with water
  3. 3
    过滤The obtained crystal was collected by filtration
  4. 4
    洗涤washed with water and 95% EtOH

实验过程

To a solution of 0.22 g of the ester described in above (1) in dioxane (2.2 ml) was added 1 N NaOH (0.9 ml). After stirring for 2 hours, the mixture was treated with 1 N hydrochloric acid (0.9 ml), and concentrated under reduced pressure. The residue was diluted with water. The obtained crystal was collected by filtration, and washed with water and 95% EtOH to give 0.15 g of the titled compound. Yield: 80%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06716605B2uspto-grants-2004_04