3,4-Dimethylbenzoyl chloride → 6-(3,4-Dimethylbenzoyl)-(6H)-dibenz[c,e][1,2]oxaphosphorin 6-oxide

HRID 2371986노트

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HRID 2371986 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5](Cl)=[O:6].C[O:13][P:14]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[C:17]2[CH:24]=[CH:25][CH:26]=[CH:27][C:16]=2[O:15]1>>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([P:14]1(=[O:13])[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[C:17]2[CH:24]=[CH:25][CH:26]=[CH:27][C:16]=2[O:15]1)=[O:6]

참가 물질

3

반응물 2

HCID 27585353,4-Dimethylbenzoyl chlorideHCID 114361486-methoxy-(6H)-dibenz[c,e][1,2]-oxaphosphorin

생성물 1

HCID 143662846-(3,4-Dimethylbenzoyl)-(6H)-dibenz[c,e][1,2]oxaphosphorin 6-oxide

반응 조건

온도
100 °C

실험 절차

50.6 g (0.3 mol) of 3,4-dimethylbenzoyl chloride were warmed to 80° C. under a nitrogen atmosphere. 69 g (0.3 mol) of 6-methoxy-(6H)-dibenz[c,e][1,2]oxaphosphorin were added dropwise while stirring. Crystallization began even during the dropwise addition, and the temperature was therefore increased to 100° C.; at the same time, an additional 100 ml of toluene were added dropwise. When the dropwise addition was complete, the mixture was heated to reflux. When the reaction was complete and after crystallization, 87 g (83% of theory) of the abovementioned compound, which had a melting point of 160° to 162° C., were obtained.

후처리

  1. customCrystallization
  2. additionbegan even during the dropwise addition
  3. additionat the same time, an additional 100 ml of toluene were added dropwise
  4. additionWhen the dropwise addition
  5. temperaturethe mixture was heated to reflux
  6. customafter crystallization, 87 g (83% of theory) of the abovementioned compound, which
  7. customwere obtained

출처 및 근거

ORD 기록
ord-62bc07d2155b4ab68c2958717c98f57d
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05096935

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