反应详情

温度

60 °C

A stirred solution of 6-bromo-1-(4-piperidinyl)-5-(trifluoromethyl)-1,3-dihydro-2H-benzimidazol-2-one (free base of D69, 0.28 g, 0.77 mmol) in N,N-dimethylacetamide (3 ml) at room temperature under argon was treated with acetone cyanohydrin (0.13 g, 1.5 mmol) and dry magnesium sulphate (0.50 g), then heated at 60° C. whilst a gentle stream of argon was passed over the well stirred mixture. After 48 hrs the mixture containing a thick pale yellow precipitate was cooled to room temperature and treated with dichloromethane (25 ml), then stirred for 15 minutes. The liquid which contained the fine suspension of the solid precipitate was decanted off from the magnesium sulphate which had settled to the base of the flask. The decanted mixture was then filtered to afford the title compound as a white solid (>90% purity) (0.24 g, 66%).

1. additionAfter 48 hrs the mixture containing a thick pale yellow precipitate
2. temperaturewas cooled to room temperature
3. stirringstirred for 15 minutes
4. additionthe fine suspension of the solid precipitate
5. customwas decanted off from the magnesium sulphate which
6. filtrationThe decanted mixture was then filtered