反应详情

温度

40 °C

To a solution of benzyl 7-(bromoacetyl)-2-oxo-2,3-dihydro-1,3-benzothiazol-4-yl carbonate (50 mg) in dry DMF (1 ml) stirring under nitrogen was added N-benzyl-6-(4-phenylbutoxy)hexan-1-amine (Tetrahedron Letters. 1994, 35, 9375) (60 mg) and N,N-diisopropylethylamine (32 μl). After stirring at 40° C. for 2 h, 2N HCl was added and the mixture extracted with ethyl acetate. The solution was dried (MgSO4), filtered and evaporated in vacuo. The residue was purified on a 5 g silica SPE cartridge, eluting with a stepped gradient of 2% to 10% methanol-dichloromethane mixtures to give the title compound (50 mg). LCMS RT=3.14 min.

1. extractionthe mixture extracted with ethyl acetate
2. dry with materialThe solution was dried (MgSO4)
3. filtrationfiltered
4. customevaporated in vacuo
5. customThe residue was purified on a 5 g silica SPE cartridge
6. washeluting with a stepped gradient of 2% to 10% methanol-dichloromethane mixtures