Azobisisobutyronitrile → 9-Cyclopentyl-9-phosphabicyclo[3.3.1]nonane 9-cyclopentyl-9-phosphabicyclo[4.2.1]nonane

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)

ORDレコード

ord-8a9efa35c8e34dfc84178de95c777e39

出典データセット

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08097691B2