N-(2-溴乙基)-4-氟苯磺酰胺

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A suspension of N-(2-Bromo-ethyl)-4-fluoro-benzenesulfonamide (7 g, 0.0179 mol; see step (i) above) and 9-oxa-3,7-diaza-bicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester (11.2 g, 0.159 mol; see WO 01/28992) and K2CO3 (9.7 g, 0.0798 mol) in dry acetonitrile (70 ml) was stirred at 60° C. overnight under nitrogen atmosphere. The reaction mixture was partitioned between brine and ethyl acetate. Organic layer was washed with brine and dried over sodium sulfate. Solvent evaporation under reduced pressure followed by column chromatography over silica gel using 7% ethyl acetate in petroleum ether as eluent afforded the sub-title compound as a solid. Yield: 4 g The reaction mixture was partitioned between brine and ethyl acetate Organic layer was washed with brine dried over sodium sulfate Solvent evaporation under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 4-Fluoro benzene sulfonyl chloride (8 g, 0.0411 mol) was added dropwise at 0° C. to a solution of 2-bromoethylamine hydrogen bromide (10.27 g, 0.0501 mol) and triethyl amine (14.3 ml, 0.1029 mol) in dry dichloromethane (100 ml) and stirred at room temperature for 1 h under nitrogen atmosphere. The reaction mixture was diluted with water and extracted with ethyl acetate. Organic layer was washed with water and brine and dried over sodium sulfate. Solvent evaporation under reduced pressure afforded the sub-title product as a liquid. Yield: 11 g extracted with ethyl acetate Organic layer was washed with water and brine dried over sodium sulfate Solvent evaporation under reduced pressure