Triethylamine → HCID 53634291, compound

HRID 1979333Notes

Reaction equation

HRID 1979333 reaction equation
[CH3:1][O:2][CH2:3][N:4]1[C:10]2[CH:11]=[C:12]([O:15][CH3:16])[CH:13]=[CH:14][C:9]=2[N:8]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:7][C:6](=[N:23][OH:24])[C:5]1=[O:25].[CH2:26]([N:29]=[C:30]=[O:31])[CH2:27][CH3:28].C(N(CC)CC)C>O1CCCC1>[CH3:1][O:2][CH2:3][N:4]1[C:10]2[CH:11]=[C:12]([O:15][CH3:16])[CH:13]=[CH:14][C:9]=2[N:8]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:7][C:6](=[N:23][O:24][C:30]([NH:29][CH2:26][CH2:27][CH3:28])=[O:31])[C:5]1=[O:25]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 61033Propyl isocyanateHCID 86756976HCID 86756976, compound

Product 1

HCID 53634291HCID 53634291, compoundYield 62.4%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

1-Methoxymethyl-2-oxo-3-hydroxyimino-5-phenyl-8-methoxy-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (1.0 g) was dissolved in tetrahydrofuran (10 ml), propyl isocyanate (0.62 g) and triethylamine (0.74 g) were added thereto, the mixture was refluxed for 2 hours and 30 minutes. The reaction mixture was allowed to cool to room temperature, crystals so precipitated were collected by filtration, and the crystals were washed with diisopropyl ether, to thereby obtain 0.78 g of the titled compound as white crystals.

Workup

  1. temperaturethe mixture was refluxed for 2 hours and 30 minutes
  2. customcrystals so precipitated
  3. filtrationwere collected by filtration
  4. washthe crystals were washed with diisopropyl ether

Sources & evidence

ORD record
ord-d481886bb1d44341b6a3921c1194ef54
Source dataset
uspto-grants-2001_05
Patent number
US06239131B1

Reaction notes

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