[Si:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15]O)=[C:11]([Cl:17])[CH:10]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C(N(CC)CC)C.CS([Cl:29])(=O)=O>ClCCl.C(OCC)(=O)C>[C:4]([Si:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][Cl:29])=[C:11]([Cl:17])[CH:10]=1)([CH3:3])[CH3:2])([CH3:7])([CH3:6])[CH3:5]To a stirred solution of tert-butyl[3-chloro-4-(chloromethyl)phenoxy]dimethylsilane (step 1, 500 mg, 1.83 mmol) in dichloromethane (5 mL) were added triethylamine (0.139 mL, 2.75 mmol) and methane sulfonylchloride (231 mg, 2.02 mmol) at room temperature. The mixture was stirred for 2 h at the same temperature. The mixture was diluted with ethyl acetate (100 mL), and the mixture was washed with water and brine, dried over sodium sulfate and evapolated. The residue was purified by silica gel (40 g) eluting with hexane/ethyl acetate (10/1) to afford 580 mg (quant.) of the title compound as a colorless oil:
Wird geladen…
