반응식
[CH3:1][P:2]1(=[O:7])[CH2:6][CH2:5][CH:4]=[CH:3]1.O=O.[CH3:10][O:11][P:12]([CH3:14])[OH:13]>>[CH3:10][O:11][P:12]([CH:3]1[CH2:4][CH2:5][CH2:6][P:2]1([CH3:1])=[O:7])([CH3:14])=[O:13]참가 물질
4
실험 절차
A total of 116 g of 1-methyl-1-oxophospholine and 6 g of tert.-butyl peroctoate in 30 g of methane phosphonous acid methyl ester are simultaneously added dropwise with stirring at 120° C to 282 g of oxygen-free methane phosphonous acid methyl ester. The reaction time is 90 minutes. Excess methane phosphonous acid methyl ester and a little 1-methyl oxophospholine are distilled off. For purification, the residue of 205 g of 1-methyl-1-oxophospholanyl methyl phosphinic acid methyl ester is distilled in vacuo (b.p. 210° -220° C) and gives 186 g of a pure product which hardens very slowly into star-shaped crystals which become liquid again at a temperature above 70° C.
후처리
- distillationExcess methane phosphonous acid methyl ester and a little 1-methyl oxophospholine are distilled off
- customFor purification
- distillationthe residue of 205 g of 1-methyl-1-oxophospholanyl methyl phosphinic acid methyl ester is distilled in vacuo (b.p. 210° -220° C)
출처 및 근거
- ORD 기록
- ord-90f8c4e4f56e479ba54f350c648879f2
- 출처 데이터셋
- uspto-grants-1977_10
- 특허 번호
- US04052484
연결된 노트
불러오는 중…