反应详情

3-Methoxypropyl-magnesium chloride was generated from 1 -chloro-3-methoxypropane (10.0 g, 92.0 mmol) and Mg metal (2.26 g, 93.0 mmol) and reacted with dichloromethylphosphine (4.1 ml, 0.46 mmol) according to General Method I. The residue was purified by fractional distillation (bp=110° C.@2.8 mm Hg) affording 5.9 g (68%) of bis(3-methoxypropyl)methylphosphine as a mobile colorless oil. 31PNMR(Benzene-d6):δ -43.3. MS (HREI) m/z=192.1279 (192.1279 calc'd for C9H21O2P).

1. distillationThe residue was purified by fractional distillation (bp=110° C.@2.8 mm Hg)