Hydrazine hydrate (1:1) → HCID 20060998, compound

HRID 1085152Notes

Reaction equation

HRID 1085152 reaction equation
[Cl:1][C:2]1[C:29]([Cl:30])=[CH:28][C:5]2[NH:6][C:7](=S)[CH2:8][C:9]([C:11]3[CH:16]=[CH:15][C:14]([N:17]4[C:25]5[CH:24]=[CH:23][N:22]=[CH:21][C:20]=5[N:19]=[C:18]4[CH3:26])=[CH:13][CH:12]=3)=[N:10][C:4]=2[CH:3]=1.O.[NH2:32][NH2:33]>C(O)CCC.CO>[Cl:1][C:2]1[C:29]([Cl:30])=[CH:28][C:5]2[N:6]=[C:7]([NH:32][NH2:33])[CH2:8][C:9]([C:11]3[CH:16]=[CH:15][C:14]([N:17]4[C:25]5[CH:24]=[CH:23][N:22]=[CH:21][C:20]=5[N:19]=[C:18]4[CH3:26])=[CH:13][CH:12]=3)=[N:10][C:4]=2[CH:3]=1

Participants

5

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 10479006HCID 10479006, compound

Product 1

HCID 20060998HCID 20060998, compound

Reagents, catalysts & solvents 2

HCID 2631-ButanolSolventHCID 887MethanolSolvent

Conditions

Temperature
100 °C

Procedure

A mixture of 7,8-dichloro-2,3-dihydro-4-[4-(2-methylimidazo[4,5-c]pyrid-1-yl)phenyl]-1H-[1,5]benzodiazepin-2-thione (452 mg, 1.0 mmol), hydrazine hydrate (100 mg, 2 mmol) and red mercuric oxide (217 mg, 1.0 mmol) in n-butanol was heated at 100° C. for 30 minutes. The mixture was diluted with methanol (300 ml), filtered through Arbocel filter aid and the filtrate was concentrated under reduced pressure. The crude product was used directly for Example 32.

Workup

  1. filtrationfiltered through Arbocel
  2. filtrationfilter aid
  3. concentrationthe filtrate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-7b0921f25ca044b891de05e8eec9087e
Source dataset
uspto-grants-1991_04
Patent number
US05008263

Reaction notes

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