反应详情

As described in Example 4, a mixture of 19.6 g of mesityl oxide (0.20 mole), 99.6 g of diisopropyl phosphite (0.60 mole) and 100 ml of benzene was reacted with 2.1 g of sodium as catalyst over the course of 10 minutes. The reaction was vigorously exothermic. After a subsequent reaction for 15 minutes at the boiling temperature, the reaction mixture was neutralized with 5.5 g of glacial acetic acid and diluted with 150 ml of benzene. After the reaction solution cooled, it was extracted with 20 ml of benzene twice, and the extract was combined with the chief portion, dried over Na2SO4 and concentrated in a rotary evaporator. The distillation yielded 27.5 g of a first fraction with a boiling point of 68°-75° C./10 mm Hg and consisting of virtually pure diisopropyl phosphite as well as 58.0 g (78.3%) of the oxaphospholane which boiled at 120°/0.02 mm Hg to 125° C./ 0.05 mm Hg; 5.3 g remained as residue.

1. customAfter a subsequent reaction for 15 minutes at the boiling temperature
2. temperatureAfter the reaction solution cooled
3. extractionit was extracted with 20 ml of benzene twice
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in a rotary evaporator
6. distillationThe distillation
7. customyielded 27.5 g of a first fraction with a boiling point of 68°-75° C./10 mm Hg