Diketene → Isobutyl methyl(2-oxo-4-oxetanylmethyl)phosphinate
反応式
[CH2:1]=[C:2]1[O:6][C:4](=[O:5])[CH2:3]1.[CH3:7][P:8]([O-:14])[O:9][CH2:10][CH:11]([CH3:13])[CH3:12]>>[CH3:7][P:8]([CH2:1][CH:2]1[O:6][C:4](=[O:5])[CH2:3]1)(=[O:14])[O:9][CH2:10][CH:11]([CH3:13])[CH3:12]参加物
3
実験手順
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.
後処理
- temperaturewas heated at 85° in a nitrogen atmosphere
- additionAfter the addition the reaction mixture
- customa wiped-wall still at a temperature of 50° C.