反应详情

温度

80 °C

A 25 ml stirred vessel was charged at room temperature under nitrogen with 2.0 g (18.5 mmol) of 1,5-cyclooctadiene (Aldrich, 82018 Taufkirchen, DE), 71 mg of azo-bis-isovaleronitrile (VAZO 67, Aldrich, 82018 Taufkirchen, DE) and 3.8 g of a 50% strength solution of monocyclopentylphosphine in toluene (Cytec). This initial charge was subsequently heated to a bath temperature of 80° C. with stirring. After 24 h it was cooled to room temperature, treated with a further 71 mg of AIBN and heated with stirring at a bath temperature of 80° C. for a further 24 h. Subsequently it was worked up by vacuum distillation, giving 2.3 g of cyclopentylphobane isomer mixture (60% of theory; b.p.: 95° C. at 0.05 mbar).

1. additionThis initial charge
2. stirringwith stirring
3. temperatureAfter 24 h it was cooled to room temperature
4. temperatureheated
5. stirringwith stirring at a bath temperature of 80° C. for a further 24 h
6. distillationSubsequently it was worked up by vacuum distillation
7. customgiving 2.3 g of cyclopentylphobane isomer mixture (60% of theory; b.p.: 95° C. at 0.05 mbar)