反应 #8912

反应方程式

acetic acid

Lithium hydroxide H2O

product

2-{[6-(2-Chlorophenyl)-5-(4-chlorophenyl)-2-(2-hydroxy-2-methylpropanoyl)furo[2,3-b]pyridin-3yl]amino}-2-oxoethyl acetate

methanol

→

title compound

N-[6-(2-Chlorophenyl)-5-(4-chlorophenyl)-2-(2-hydroxy-2-methylpropanoyl)furo[2,3-b]pyridin-3-yl]-2-hydroxyacetamide

溶剂

THF

反应条件

后处理

1. 1
   浓缩the solution concentrated
2. 2
   workup.ADDITIONThe residue was diluted with ethyl acetate
3. 3
   洗涤this solution washed two times with aqueous sodium bicarbonate
4. 4
   浓缩The solution was concentrated
5. 5
   其他purified via flash chromatography on silica gel with a gradient elution of 0 to 55% ethyl acetate in methylene chloride
6. 6
   其他The product was then further purified by recrystallization from ethanol

实验过程

Lithium hydroxide-H2O (0.293 g), the product of Step A (3.78 g), and methanol (8.4 mL) were combined in 245 mL of THF and stirred at room temperature. After 5 min 0.50 mL of acetic acid was added and the solution concentrated. The residue was diluted with ethyl acetate and this solution washed two times with aqueous sodium bicarbonate. The solution was concentrated and purified via flash chromatography on silica gel with a gradient elution of 0 to 55% ethyl acetate in methylene chloride. The product was then further purified by recrystallization from ethanol to afford the title compound. HPLC/MS: 499.0 (M+1), 500.8 (M+3); Rt=3.77 min.

来源