反应详情

温度

0 °C

A solution of 600 mg of the compound of EXAMPLE 1 in 24 ml of DCM is added dropwise to a solution of 0.19 ml of diethylamino sulfide trifluoride in 24 ml of DCM at -78° C. under nitrogen. The mixture is allowed to warm up slowly to 0° C. and then stirred for one hour at 0° C. The reaction mixture is poured into saturated NaHCO3 solution and then extracted with DCM, washed with saturated NaCl solution and dried over MgSO4. The residue is chromatographed on fine silica using AcOEt/toluene (5/95 to 40/60; v/v) as the eluent to give 250 mg of the expected product, m.p.=184° C.

1. extractionextracted with DCM
2. washwashed with saturated NaCl solution
3. dry with materialdried over MgSO4
4. customThe residue is chromatographed on fine silica