反应详情

To a yellow solution of 2-(5-methyl-2-p-tolylthiazol-4-yl)ethanol (200 mg, 857 μmol) in dichloromethane (3 mL) was added N,N-diisopropylethylamine (166 mg, 225 μL, 1.29 mmol) at RT. Methanesulfonyl chloride (113 mg, 76.8 μL, 986 μmol) was added at 0-5° C. and stirring was continued for 4 h at 0° C. The reaction mixture was poured into ethyl acetate (25 mL) and extracted with KHSO4 (10% aqueous solution, 15 mL). The organic phase was washed with water (2×15 mL) and brine (1×20 mL). The aqueous layers were back-extracted with ethyl acetate (1×25 mL) and the combined organic layer was dried over MgSO4 and concentrated in vacuo to give 280 mg (99%) of yellow oil which was used without further purification for the next step.

1. extractionextracted with KHSO4 (10% aqueous solution, 15 mL)
2. washThe organic phase was washed with water (2×15 mL) and brine (1×20 mL)
3. extractionThe aqueous layers were back-extracted with ethyl acetate (1×25 mL)
4. dry with materialthe combined organic layer was dried over MgSO4
5. concentrationconcentrated in vacuo