تفاعل #595355

معادلة التفاعل

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

المذيبات

1,2-dimethoxyethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةafter cooling, at RT for a further 10 h
2. 2
   أخرىThe precipitate formed
3. 3
   ترشيحis filtered off with suction
4. 4
   غسيلwashed once with about 2 ml of cold water
5. 5
   أخرىThis 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)

الإجراء التجريبي

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).

المصدر