Phenyl isocyanate → HCID 12785880, compound

HRID 1075212Notes

Reaction equation

HRID 1075212 reaction equation
[C:1](=[O:4])(O)[O-:2].[Na+].[Cl-].O[NH3+:8].[Cl:9][C:10]1[CH:11]=[CH:12][C:13]2[NH:19][C:18](=S)[CH2:17][N:16]=[C:15]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[F:27])[C:14]=2[CH:28]=1.[C:29]1([N:35]=C=O)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>O1CCOCC1.CN(C)C=O.C(O)(C)C>[Cl:9][C:10]1[CH:11]=[CH:12][C:13]2[N:19]=[C:18]([NH:8][O:2][C:1](=[O:4])[NH:35][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[CH2:17][N:16]=[C:15]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[F:27])[C:14]=2[CH:28]=1

Participants

8

Reactant 4

HCID 7672Phenyl isocyanateHCID 21645Hydroxylamine HCl2×HCID 516892Sodium Bicarbonate2×HCID 3081966N-Desmethylquazepam

Product 1

HCID 12785880HCID 12785880, compound

Reagents, catalysts & solvents 3

HCID 3776IsopropanolSolventHCID 6228DimethylformamideSolventHCID 312751,4-DioxaneSolvent

Procedure

0.6 g of sodium bicarbonate and 0.5 g of hydroxylammonium chloride are added to 2 g of 7-chloro-5-(2-fluorophenyl)-1,3-dihydro-2H-1,4-benzodiazepine-2-thione in 40 ml of dioxane and 20 ml of dimethylformamide and the mixture is stirred for 8 hours at room temperature. Further addition of 0.2 g of sodium bicarbonate and 0.2 g of hydroxylammonium chloride, stirring for 1/2 hour at 50° C. and addition of 0.8 ml of phenylisocyanate yields, after the usual working up process, 0.7 g of colorless crystals of melting point 126° to 128° C. (from isopropanol).

Workup

  1. stirringstirring for 1/2 hour at 50° C.
  2. customyields

Sources & evidence

ORD record
ord-ad66bd358886461987a0a2e48c7729e6
Source dataset
uspto-grants-1983_07
Patent number
US04395409

Reaction notes

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