Phenyl isocyanate → HCID 12785879, compound

HRID 1075210Notes

Reaction equation

HRID 1075210 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[NH:12][C:11](=S)[CH2:10][N:9]=1.[C:23](=[O:26])(O)[O-:24].[Na+].[Cl-].O[NH3+:30].[C:31]1([N:37]=C=O)[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[N:12]=[C:11]([NH:30][O:24][C:23](=[O:26])[NH:37][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH2:10][N:9]=1

Participants

5

Reactant 4

HCID 7672Phenyl isocyanateHCID 21645Hydroxylamine HClHCID 516892Sodium BicarbonateHCID 12371433HCID 12371433, compound

Product 1

HCID 12785879HCID 12785879, compound

Procedure

2 g of 5-(2-chlorophenyl)-7-nitro-1,3-dihydro-2H-1,4-benzodiazepine-2-thione are reacted with 0.8 g of sodium bicarbonate and 0.7 g of hydroxylammonium chloride, analogously to Example 16. After stirring for 8 hours at room temperature, 0.8 ml of phenyl isocyanate are added, and the mixture is stirred for 1/2 an hour and precipitated with water; the oil produced is crystallized by means of ethanol. Recrystallization from ethanol yields 2 g of yellow crystals of melting point 201° to 203° C.

Workup

  1. stirringthe mixture is stirred for 1/2 an hour
  2. customprecipitated with water
  3. customthe oil produced
  4. customis crystallized by means of ethanol
  5. customRecrystallization from ethanol

Sources & evidence

ORD record
ord-dd794fd9ec6e43c0b9ff3392f8554cb1
Source dataset
uspto-grants-1983_07
Patent number
US04395409

Reaction notes

Loading…