Triphenylphosphine → HCID 19438781, compound

HRID 1733882Notes

Reaction equation

HRID 1733882 reaction equation
C(O[C:4]([NH:6][NH:7][C:8]1[C:9](=[O:29])[N:10](O)[C:11]2[C:16]([N:17]=1)=[CH:15][C:14]([N:18]1[CH:22]=[CH:21][N:20]=[C:19]1[CH3:23])=[C:13]([C:24]([F:27])([F:26])[F:25])[CH:12]=2)=[O:5])C.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>CN(C)C=O>[CH3:23][C:19]1[N:18]([C:14]2[CH:15]=[C:16]3[C:11]([NH:10][C:9](=[O:29])[C:8]4[N:17]3[C:4](=[O:5])[NH:6][N:7]=4)=[CH:12][C:13]=2[C:24]([F:25])([F:26])[F:27])[CH:22]=[CH:21][N:20]=1

Participants

4

Reactant 2

HCID 11776TriphenylphosphineHCID 19438762HCID 19438762, compound

Product 1

HCID 19438781HCID 19438781, compoundYield 82.4%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

To a solution of 1 g crude 3-(2-ethoxycarbonylhydrazino)-1-hydroxy-6-(2-methyl-1H-imidazol-1-yl)-7-trifluoromethylquinoxalin-2(1H)-one in 50 ml dry N,N-dimethylformamide was added 1.05 g (~4.0 mmol) triphenylphosphine. Stirring was continued at 130° C. for 17 h followed by evaporation in vacuo. Column chromatography (silica gel; eluent: dichloromethane containing 10% methanol) gave the title compound (0.7 g; 75%). M.p. 375° C. (decomp.).

Workup

  1. customfollowed by evaporation in vacuo

Sources & evidence

ORD record
ord-286a455eac124bd3aeb14c2c4f80d0b4
Source dataset
uspto-grants-1996_07
Patent number
US05532236

Reaction notes

Loading…