反应详情

温度

85 °C

A solution of 0.98 parts of bis-(t-butylcyclohexyl)perdicarbonate in 12.6 parts of diketene was added dropwise over 1 hour to 90.2 parts of n-butyl ethylphosphonite which was vigorously stirred at 85° C. in a nitrogen atmosphere. After the addition the reaction mixture was passed down a wiped wall still at a temperature of 50° C. and a pressure of 0.13 mb to remove the excess phosphonite. The residue was distilled on the wiped wall still at a temperature of 75° C. and a pressure of 0.013 mb. The product n-butyl ethyl(2-oxo-4-oxetanylmethyl)phosphinate, was obtained as a colourless oil which the 31P NMR showed to be a nearly equal mixture of diastereoisomers having chemical shifts of δ-52.4 and δ-52.7 and which had the following elemental analysis by weight.

1. additionAfter the addition the reaction mixture
2. customstill at a temperature of 50° C.
3. customa pressure of 0.13 mb to remove the excess phosphonite
4. distillationThe residue was distilled on the wiped wall still at a temperature of 75° C.