反应详情

A mixture of 4.2 parts of diketene and 0.33 parts of bis-(t-butylcyclohexyl)perdicarbonate was added dropwise over 1 hour to 27.2 parts of vigorously stirred isobutyl methylphosphonite which was heated at 85° 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° and a pressure of 0.13 mb. The product isobutyl methyl(2-oxo-4-oxetanylmethyl)phosphinate was obtained as a colourless oil with a characteristic infra-red band at 1820 cm-1.

1. temperaturewas heated at 85° in a nitrogen atmosphere
2. additionAfter the addition the reaction mixture
3. customa wiped-wall still at a temperature of 50° C.
4. customa pressure of 0.13 mb to remove the excess phosphonite
5. distillationThe residue was distilled on the wiped wall still at a temperature of 75°