반응식
[CH3:1][O:2][P:3](C1C=CC=CC=1)[O:4]C.CI.P([O-])[O-].[C:17]1([CH3:23])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>>[C:17]1([CH2:23][PH:3](=[O:4])[O:2][CH3:1])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1참가 물질
반응 조건
- 온도
- 110 °C
실험 절차
To a suitable vessel equipped with a stirring means, a temperature measuring means and a material addition means was charged 11 parts dimethylphenylphosphonite, 2.5 parts methyl iodide and 9 parts toluene. The resultant solution was slowly heated. The reaction is exothermic and the temperature increases to about 110° C., the reaction mixture is maintained at a temperature of about 100°-120° C., and an additional 185 parts dimethylphenylphosphonite slowly added. Additional amounts of methyl iodide, in about 1 part increments, are occasionally added during the phosphonite addition. The reaction mixture was maintained at about 110° C. for an additional hour following the addition of components. The reaction mixture was then distilled collecting the portion boiling at 148°-149° C./17 mm. (96 percent yield of methyl phenylmethylphosphinate). [Harwood and Grisley J. Am. Chem. Soc., 82, 423 (1960)]. ##STR3##
후처리
- customTo a suitable vessel equipped with a stirring means
- additiona material addition means
- temperaturethe reaction mixture is maintained at a temperature of about 100°-120° C.
- temperatureThe reaction mixture was maintained at about 110° C. for an additional hour
- additionthe addition of components
- distillationThe reaction mixture was then distilled
- customcollecting the portion boiling at 148°-149° C./17 mm
출처 및 근거
- ORD 기록
- ord-5e28e03566ac40e9abf270423643f366
- 출처 데이터셋
- uspto-grants-1977_01
- 특허 번호
- US04005127
연결된 노트
불러오는 중…