反应 #595363

反应方程式

potassium tert-butoxide

compound

[2-(4-Chlorophenyl)-1,3-oxazol-4-yl]methanol

compound

2-Amino-4-[4-(2-hydroxyethoxy)phenyl]-6-(phenylsulfanyl)pyridine-3,5-dicarbonitrile

water

→

product

2-Amino-6-{[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methoxy}-4-[4-(2-hydroxyethoxy)phenyl]-pyridine-3,5-dicarbonitrile

溶剂

acetic acid

1,2-dimethoxyethane

反应条件

后处理

1. 1
   温度cooled to RT
2. 2
   workup.STIRRINGstirred at this temperature for a further 8 h
3. 3
   其他A precipitate is formed
4. 4
   过滤which is filtered off with suction
5. 5
   其他purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)
6. 6
   其他Removal of the solvent
7. 7
   其他on a rotary evaporator

实验过程

72 mg (0.64 mmol) of potassium tert-butoxide are suspended in 1 ml of dry 1,2-dimethoxyethane. In succession, 270 mg (1.29 mmol) of the compound from Example 100A and 50 mg (0.13 mmol) of the compound from Example 99A are then added. The reaction mixture is stirred at 60° C. for 2 h and then cooled to RT and stirred at this temperature for a further 8 h. 5 ml of water and 1 ml of 2 N acetic acid are then added to the mixture. A precipitate is formed, which is filtered off with suction and purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5). Removal of the solvent on a rotary evaporator gives the product as a yellow solid.

来源