反应详情

The subtitle compound was prepared from 3-amino-4-cyano-5-(2,2,2-trifluoroethoxy)-anisole and 1-acetyl-4-(4-morpholinecarbonyl)-1,4-diazepane following a similar procedure to that described in Example 10(g) allowing the reaction to stir for 60 hours at room temperature. The crude product was purified on silica gel eluting with a solvent gradient of dichloromethane:methanol (100:0 to 95:5, v/v). The product was dissolved in a minimum volume of dichloromethane and an excess of ethereal hydrogen chloride added. The resulting precipitate was filtered off and partitioned between saturated aqueous sodium hydroxide solution (100 ml ) and dichloromethane (200 ml). The organic layer was dried (MgSO4) and evaporated under reduced pressure to give the subtitle compound (1.83 g, 95%). Rf 0.58 (dichloromethane:methanol:0.880 aqueous ammonia 92:7:1, v/v). MS m/z 484 (MH)+.

1. customthe reaction
2. customThe crude product was purified on silica gel eluting with a solvent gradient of dichloromethane:methanol (100:0 to 95:5
3. dissolutionThe product was dissolved in a minimum volume of dichloromethane
4. additionan excess of ethereal hydrogen chloride added
5. filtrationThe resulting precipitate was filtered off
6. custompartitioned between saturated aqueous sodium hydroxide solution (100 ml ) and dichloromethane (200 ml)
7. dry with materialThe organic layer was dried (MgSO4)
8. customevaporated under reduced pressure