反应详情

温度

85 °C

A mixture of 13.2 parts of dodecyl methylphosphite, 4.2 parts of diketene and 0.6 parts of bis-(t-butylcyclohexyl)-perdicarbonate was added dropwise over 30 minutes to 39.6 parts of dodecylmethylphosphite which was vigorously stirred at 85° C. in a nitrogen atmosphere. On completion of the addition the reaction mixture was heated for a further 30 minutes at 85° C., then the excess of dodecylmethylphosphite was removed on a wiped wall still at a wall temperature of 80° C. and pressure 0.013 mb. The residue was distilled on a wiped wall still at a wall temperature of 150° C. and pressure 0.013 mb, and gave dodecyl methyl 2-oxo-4-oxetanylmethylphosphonate as a colourless oil which had the following analysis by weight:

1. additionOn completion of the addition the reaction mixture
2. temperaturewas heated for a further 30 minutes at 85° C.
3. customthe excess of dodecylmethylphosphite was removed on a wiped wall still at a wall temperature of 80° C. and pressure 0.013 mb
4. distillationThe residue was distilled on a wiped wall still at a wall temperature of 150° C. and pressure 0.013 mb