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

HRID 2371986Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2371986
[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]

Komponenten

3

Edukt 2

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

Produkt 1

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

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-62bc07d2155b4ab68c2958717c98f57d
Quelldatensatz
uspto-grants-1992_03
Patentnummer
US05096935

Notizen zur Reaktion

Wird geladen…