반응 #595355

반응 방정식

water

potassium tert-butoxide

compound

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

compound

2-Amino-4-(4-{[(4S)-2,2-dimethyl-1,3-dioxolan-4-yl]methoxy}-phenyl)-6-(phenylthio)pyridine-3,5-dicarbonitrile

→

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

용매

1,2-dimethoxyethane

반응 조건

후처리

1. 1
   온도after cooling, at RT for a further 10 h
2. 2
   기타The precipitate formed
3. 3
   여과is filtered off with suction
4. 4
   세척washed once with about 2 ml of cold water
5. 5
   기타This is followed by purification by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)

실험 절차

122 mg (1.09 mmol) of potassium tert-butoxide are suspended in 2 ml of dry 1,2-dimethoxyethane. 229 mg (1.09 mmol) of the compound from Example 100A and 100 mg (0.22 mmol) of the compound from Example 98A are then added successively. The reaction mixture is stirred at 60° C. for 2 h and, after cooling, at RT for a further 10 h. 5 ml of water are then added to the mixture. The precipitate formed is filtered off with suction and washed once with about 2 ml of cold water. This is followed by purification by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5).

출처