Toluene → HCID 178502922, 화합물

HRID 1415450

반응식

HRID 1415450 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]=1

참가 물질

5

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

  1. customTo a suitable vessel equipped with a stirring means
  2. additiona material addition means
  3. temperaturethe reaction mixture is maintained at a temperature of about 100°-120° C.
  4. temperatureThe reaction mixture was maintained at about 110° C. for an additional hour
  5. additionthe addition of components
  6. distillationThe reaction mixture was then distilled
  7. 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

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