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

HRID 2371986ノート

反応式

HRID 2371986 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

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

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-62bc07d2155b4ab68c2958717c98f57d
出典データセット
uspto-grants-1992_03
特許番号
US05096935

反応ノート

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