Methoxydiphenylphosphine → 2,4,6-Trimethylbenzoyl diphenylphosphine oxide

HRID 851516

Reaction equation

C[O:2][P:3]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH3:16][C:17]1[CH:25]=[C:24]([CH3:26])[CH:23]=[C:22]([CH3:27])[C:18]=1[C:19](Cl)=[O:20]>CCOCC>[CH3:16][C:17]1[CH:25]=[C:24]([CH3:26])[CH:23]=[C:22]([CH3:27])[C:18]=1[C:19]([P:3](=[O:2])([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[O:20]

Participants

Conditions

Temperature: 50 °C

Procedure

648 parts of methoxydiphenylphosphine are added slowly to 547.5 parts of 2,4,6-trimethylbenzoyl chloride at 50°-95° C. in a stirred apparatus equipped with a reflux condenser and dropping funnel. The mixture is then stirred for 4-5 hours at 50° C., the contents of the flask are dissolved in ether at 30° C., and petroleum ether is added until the mixture starts to turn cloudy. On cooling, 910 parts (87% of theory) of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide crystallize. Pale yellow crystals, melting point 89°-92° C.

Workup

customequipped with a reflux condenser
temperatureOn cooling
custom910 parts (87% of theory) of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide crystallize

Sources & evidence

ORD record: ord-2c6d51c9b77545f29888bf4911cdb0d0
Source dataset: uspto-grants-1983_05
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04385109

Linked notes

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