1-phenyl-2-trimethylsilyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide → 1-phenyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide

HRID 2058902Notes

Reaction equation

[C:1]1([P:7]2(=[O:20])[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[CH2:9][N:8]2[Si](C)(C)C)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>CO>[C:1]1([P:7]2(=[O:20])[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[CH2:9][NH:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

Conditions

Temperature: 26 °C

Procedure

The 1-phenyl-2-trimethylsilyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide was dissolved in 50 ml. of methanol and heated at reflux for 4 hours. After stirring for 16 hours at 26° C., the resulting solution was concentrated in vacuo and the residue was crystallized from ethyl acetate to yield 1-phenyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide (9.0 g, 33% yield) as a white solid having a melting point of 177°-180° C. and the following analysis:

Workup

temperatureat reflux for 4 hours
concentrationthe resulting solution was concentrated in vacuo
customthe residue was crystallized from ethyl acetate

Sources & evidence

ORD record: ord-40439cfb11984cbda2e1f10118655e30
Source dataset: uspto-grants-1982_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04319913

Reaction notes

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