反应详情

温度

2.5 °C

To an ice cooled suspension of sodium hydride (60-65% in mineral oil, 0.030 g) in absolute DMSO (3 ml) was added 4-(4-amino-3-methanesulfonyl-phenyl)-piperidine-1-carboxylic acid tert-butyl ester (0.106 g). The mixture was stirred at 0-5° C. for 30 minutes, and a solution 5-fluoro-3-methylbenzo[b]thiophene-2-sulphonyl chloride (0.237 g) in absolute DMSO (1 ml) was added dropwise. The reaction mixture was stirred at rt for 5 h, quenched with ice/water/1 N HCl, and extracted with ethyl acetate. The organic phases were washed, dried and concentrated, and the residue was chromatographed over silica gel using heptane/ethyl acetate as eluent to obtain the desired compound (0.0.025 g) methylbenzo[b]thiophene-2-sulphonyl chloride (0.237 g) to obtain the desired compound (0.025 g) as a yellowish foam. MS (ISN): 581.3 (M−H)−

1. stirringThe reaction mixture was stirred at rt for 5 h
2. customquenched with ice/water/1 N HCl
3. extractionextracted with ethyl acetate
4. washThe organic phases were washed
5. customdried
6. concentrationconcentrated
7. customthe residue was chromatographed over silica gel