反应详情

A solution of 3.03 grams (18.0 mmol) of 2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane in 10 ml of tetrahydrofuran is added over ten minutes to a solution of 8.00 grams (18.0 mmol ) of 4-dodecylamino-1-alpha-methylbenzyloxy2,2,6,6-tetramethylpiperidine, 1.91 grams (18.9 mmol) of triethylamine, and 25 ml of tetrahydrofuran. The reaction temperature increases from 20° C. to 30° C. during the addition, and triethylamine hydrochloride precipitates from solution. The reaction mixture is stirred at ambient temperature for two hours. The precipitate is removed by filtration, and the filtrate is concentrated at reduced pressure. Residual volatiles are removed by Kugelrohr distillation (at 100° C./0.2 mm) to afford 10.1 grams (97% yield) of the title compound as a viscous oil.

1. customprecipitates from solution
2. customThe precipitate is removed by filtration
3. concentrationthe filtrate is concentrated at reduced pressure
4. customResidual volatiles are removed by Kugelrohr distillation (at 100° C./0.2 mm)