反应详情

1,3-Benzenediol (5 g, 45 mmol) in dichloromethane (150 mL) was treated with chloro(t-butyl)dimethylsilane (7.5 g, 50 mmol) and triethylamine (5 g, 50 mmol). The resulting mixture was stirred at rt for 16 h then concentrated in vacuo and the residue was partitioned between ethyl acetate and water. The organic phase was washed with 6N NaOH, then concentrated in vacuo. The residue was purified by column chromatography eluting with 20% ethyl acetate in hexane to afford the title compound (4.3 g, 42%). MS (ES+) m/e 225 [M+H]+.

1. concentrationthen concentrated in vacuo
2. customthe residue was partitioned between ethyl acetate and water
3. washThe organic phase was washed with 6N NaOH
4. concentrationconcentrated in vacuo
5. customThe residue was purified by column chromatography
6. washeluting with 20% ethyl acetate in hexane