反应详情

Thionyl chloride (20 mL) was added to a solution of 14 (20.0 g, 93.6 mmol) in i-PrOH (160 mL) at 0° C. slowly. The reaction mixture was refluxed for 4 h, then cooled and concentrated. The residue was treated with ether (200 mL). The resulting ppt was collected by filtration, washed with ether, and air-dried to provide 16 as a white solid (19.7 g, 82%). 1H NMR (400 MHz, DMSO-d6) δ 8.78 (br s, 3H), 5.00 (m, 1H), 4.14 (t, 1H), 3.03 (m, 2H), 1.29 (s, 9H), 1.26 (d, 3H), 1.24 (d, 3H).

1. temperatureThe reaction mixture was refluxed for 4 h
2. temperaturecooled
3. concentrationconcentrated
4. additionThe residue was treated with ether (200 mL)
5. filtrationThe resulting ppt was collected by filtration
6. washwashed with ether
7. customair-dried