3,5-Dimethoxybenzoyl chloride → HCID 14366289, compound

HRID 2371990Notes

Reaction equation

HRID 2371990 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:12][CH3:13])[CH:11]=1)[C:6](Cl)=[O:7].C[O:15][P:16]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[C:19]2[CH:26]=[CH:27][CH:28]=[CH:29][C:18]=2[O:17]1>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:12][CH3:13])[CH:11]=1)[C:6]([P:16]1(=[O:15])[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[C:19]2[CH:26]=[CH:27][CH:28]=[CH:29][C:18]=2[O:17]1)=[O:7]

Participants

4

Reactant 2

HCID 870033,5-Dimethoxybenzoyl chlorideHCID 114361486-methoxy-(6H)-dibenz[c,e][1,2]-oxaphosphorin

Product 1

HCID 14366289HCID 14366289, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
115 °C

Procedure

35.1 g (0.175 mol) of 3,5-dimethoxybenzoyl chloride were warmed to 80° C. under a nitrogen atmosphere. 40.3 g (0.175 mol) of 6-methoxy-(6H)-dibenz[c,e][1,2]oxaphosphorin were added dropwise over the course of one hour while stirring. At the same time, the temperature was gradually increased to 115° C. When the reaction was complete, 60 ml of toluene were added at 80° C. After crystallization, 49 g (74% of theory) of the abovementioned compound of melting point 140° to 142° C. were obtained.

Workup

  1. customAfter crystallization, 49 g (74% of theory) of the abovementioned compound of melting point 140° to 142° C.
  2. customwere obtained

Sources & evidence

ORD record
ord-3a2506d8d5a542ed9c236a04227451b0
Source dataset
uspto-grants-1992_03
Patent number
US05096935

Reaction notes

Loading…