2,4-Dimethylbenzoyl chloride → HCID 14366282, compound

HRID 2371985Notes

Reaction equation

HRID 2371985 reaction equation
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].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:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]([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:5]

Participants

3

Reactant 2

HCID 1408672,4-Dimethylbenzoyl chlorideHCID 114361486-methoxy-(6H)-dibenz[c,e][1,2]-oxaphosphorin

Product 1

HCID 14366282HCID 14366282, compound

Conditions

Temperature
135 °C

Procedure

33.7 g (0.2 mol) of 2,4-dimethylbenzoyl chloride were warmed to 80° C. under a nitrogen atmosphere. 46 g (0.2 mol) of 6-methoxy-(6H)-dibenz[c,e][1,2]oxaphosphorin were added dropwise with stirring. The batch began to crystallize even during the addition. The temperature was then slowly increased to 135° C. with the proviso that toluene was added as diluent at 90° C. After digestion with toluene, 58 g (83% of theory) of the abovementioned compound of melting point 166° C. were obtained from the crystallizate.

Workup

  1. customto crystallize even during the addition
  2. additionwas added as diluent at 90° C
  3. customAfter digestion with toluene, 58 g (83% of theory) of the abovementioned compound of melting point 166° C. were obtained from the crystallizate

Sources & evidence

ORD record
ord-b0b5a7d801704cf1b9e7227d4cf57770
Source dataset
uspto-grants-1992_03
Patent number
US05096935

Reaction notes

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