(甲氧基甲基)二苯基氧化膦

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a freshly prepared tetrahydrofuran (300 mL) solution of lithium diisopropylamide (0.19 mol) under nitrogen at 0° C. was added dropwise in 30 minutes a tetrahydrofuran (200 mL) solution of diphenyl(methoxymethyl)phosphinoxide (49.5 g, 0.2 mol). After stirring for 15 minutes at 0° C., a tetrahydrofuran (100 mL) solution of 2,2-dimethylpent-4-enal (24.5 g, 0.22 mol) was added dropwise in 20 minutes to the cherry-colored mixture. After 15 minutes, the mixture was warmed to room temperature and then refluxed for 5 hours. The mixture was cooled to room temperature, charged with water (20 mL), and cooled at 0° C. under vigorous stirring. The resulting solid was filtered, washed with hexanes, and discarded. The filtrates were collected and distilled at 101-102° C. (155 mmHg) to give the title compound as a colorless oil. After 15 minutes the mixture was warmed to room temperature refluxed for 5 hours The mixture was cooled to room temperature cooled at 0° C. under vigorous stirring The resulting solid was filtered washed with hexanes The filtrates were collected distilled at 101-102° C. (155 mmHg)