反应详情

To a solution of 5-(2-fluoro-phenyl)-5-trifluoromethyl-[1,4]oxazepan-3-one (1.19 g, 4.29 mmol) in 15 mL THF was added Lawesson's reagent (955 mg, 2.36 mmol). The reaction mixture was stirred at room temperature over night. The mixture was then partitioned between aqueous Na2CO3 solution (2 mol/L) and TBME. The layers were separated, washed with aqueous Na2CO3 solution (2 mol/L), brine and TBME. The combined organic layers were dried over MgSO4.H2O and evaporated. The crude product was purified on a silica gel column by eluting with hexane/EtOAc 95/5->90/10 to give 1.25 g of the title compound as a yellow resin.

1. customThe mixture was then partitioned between aqueous Na2CO3 solution (2 mol/L) and TBME
2. customThe layers were separated
3. washwashed with aqueous Na2CO3 solution (2 mol/L), brine and TBME
4. dry with materialThe combined organic layers were dried over MgSO4.H2O
5. customevaporated
6. customThe crude product was purified on a silica gel column
7. washby eluting with hexane/EtOAc 95/5->90/10