反应详情

温度

-15 °C

Thionyl chloride (809 mg, 6.8 mmoles) in ice cold dry dichloromethane (7 ml) is added to a solution of dimethylamino pyridine (903 mg, 7.4 mmoles) in dichloromethane (15 ml) kept under nitrogen and cooled at -15° C. The oxime 34 (1.04 g, 6.2 mmoles), dissolved in dichloromethane (20 ml) is added, followed by addition of dimethyl aminopyridine as a solid (903 mg, 7.4 mmoles). The reaction mixture is then allowed to rise to room temperature, kept at 25° C. for 1 hour, diluted with dichloromethane, washed with 1N HCl, and finally with water. Concentration of the organic phase, previously dried over sodium sulfate, (30° C., 100 mm Hg) affords the title compound (620 mg) which is purified by bulb to bulb distillation (50° C., 30 mm Hg): 485 mg (52%).

1. additionis added
2. customto rise to room temperature
3. washwashed with 1N HCl
4. dry with materialConcentration of the organic phase, previously dried over sodium sulfate, (30° C., 100 mm Hg)