反应详情

温度

0 °C

To 468 mg (5.5 mmol) of 2-pyrrolidone (Fluka, Buchs, Switzerland) in 10 ml of DMF at 0° C. are added 240 mg (5.5 mmol) of 55% NaH in oil. The reaction mixture is stirred for 30 min at 0° C. and for 30 min at rt. After this time, 795 mg (5 mmol) of 3,4-difluoronitrobenzene (Aldrich, Buchs, Switzerland) are added and the reaction mixture is stirred for 1 h at rt. The reaction mixture is quenched with 1 M aqueous HCl and extracted with EtOAc (2×). The organic layers are washed with aqueous sat. NaHCO3 and with brine (3×), dried over MgSO4, filtered and evaporated. The residue is purified by flash chromatography on silica gel (hexane-EtOAc 5:1 to 1:3) to give the title compound as a solid. ES-MS: 225 (M+H)+; analytical HPLC: tret=2.99 minutes (Grad 1).

1. stirringthe reaction mixture is stirred for 1 h at rt
2. customThe reaction mixture is quenched with 1 M aqueous HCl
3. extractionextracted with EtOAc (2×)
4. washThe organic layers are washed with aqueous sat. NaHCO3 and with brine (3×)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated
8. customThe residue is purified by flash chromatography on silica gel (hexane-EtOAc 5:1 to 1:3)