3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine → 11H-s-triazolo[3,4-b][3]benzazepine

HRID 26501Notes

Reaction equation

HRID 26501 reaction equation
CS[C:3]1[N:12]2[C:6]([CH2:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[CH:10]=[CH:11]2)=[N:5][N:4]=1>C(O)C.[Ni]>[N:5]1[N:4]=[CH:3][N:12]2[CH:11]=[CH:10][C:9]3[CH:13]=[CH:14][CH:15]=[CH:16][C:8]=3[CH2:7][C:6]=12

Participants

4

Reactant 1

HCID 213234063-methylthio-11H-s-triazolo[3,4-b][3]benzazepine

Product 1

HCID 2122343511H-s-triazolo[3,4-b][3]benzazepine

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 702EthanolSolvent

Procedure

To 1.15 g of 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine in 20 ml of ethanol was added 6 ml of Raney nickel (wet) and the mixture was refluxed for 15 minutes under stirring. The Raney nickel was filtered off and the solvent was removed from the filtrate. To the residue was added water. By this procedure was obtained 11H-s-triazolo[3,4-b][3]benzazepine as crystals. Recrystallization from ethanol-n-hexane yielded colorless needles, m.p. 157°-158° C. The infrared absorption spectrum was identical with the spectrum of the same compound obtained by reacting 2-hydrazino-3-benzazepine with ortho-formic acid ester.

Workup

  1. temperaturethe mixture was refluxed for 15 minutes
  2. filtrationThe Raney nickel was filtered off
  3. customthe solvent was removed from the filtrate
  4. additionTo the residue was added water

Sources & evidence

ORD record
ord-0e51d84098784866b6379c338ba69455
Source dataset
uspto-grants-1979_04
Patent number
US04150139

Reaction notes

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