反应详情

Sodium tert-butoxide (2.55 g, 26.5 mmol) is added to a mixture of 1-((4-cyanophenyl)-(2-ethoxy-6-oxocyclohex-1-enyl)methyl)-3-(3-(trifluoromethyl)phenyl)urea (intermediate 5, 10.1 g, 22.1 mmol) and acetonitrile (100 mL). After 20 min the mixture is filtered and the precipitate is washed with acetonitrile and methyl tert-butyl ether. The precipitate is mixed with water (300 mL) and the suspension is stirred for 1 h. The precipitate is filtered again and dried under reduced pressure. Yield: 5.24 g; ESI mass spectrum [M+H]+=412; Retention time HPLC: 0.88 min (Z018_S04).

1. filtrationAfter 20 min the mixture is filtered
2. washthe precipitate is washed with acetonitrile and methyl tert-butyl ether
3. additionThe precipitate is mixed with water (300 mL)
4. filtrationThe precipitate is filtered again
5. customdried under reduced pressure
6. custom0.88 min (Z018_S04)