Perchloric Acid → 6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine-1-carboxaldehyde-diethylacetal perchlorate

HRID 268030Notes

Reaction equation

HRID 268030 reaction equation
[Cl:1]([OH:5])(=[O:4])(=[O:3])=[O:2].[CH2:6]([O:8][CH:9]([O:31][CH2:32][CH3:33])[C:10]1[N:14]2[C:15]3[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][C:16]=3[C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[N:18][CH2:19][C:13]2=[N:12][N:11]=1)[CH3:7]>CC(C)=O.CO>[CH2:32]([O:31][CH:9]([O:8][CH2:6][CH3:7])[C:10]1[N:14]2[C:15]3[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][C:16]=3[C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[N:18][CH2:19][C:13]2=[N:12][N:11]=1)[CH3:33].[Cl:1]([O-:5])(=[O:4])(=[O:3])=[O:2]

Participants

5

Reactant 2

HCID 24247Perchloric AcidHCID 215531066-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine-1-carboxaldehyde-diethylacetal

Product 1

HCID 1317100996-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine-1-carboxaldehyde-diethylacetal perchlorate

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 887MethanolSolvent

Procedure

An amount of 0.13 g (0.0013 mole) of perchloric acid is added to a solution of 0.5 g (0.00126 mole) of 6-phenyl-8-chloro-4H-s-triazolo[4,3 -a][1,4]benzodiazepine-1-carboxaldehyde-diethylacetal in 3 ml each of acetone and methanol. The salt crystallises out after the addition of 5 ml of petroleum ether. Filtration under suction is then performed and 6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine-1-carboxaldehyde-diethylacetal-perchlorate obtained, which decomposes at 250°-265°.

Workup

  1. customThe salt crystallises out
  2. additionafter the addition of 5 ml of petroleum ether
  3. filtrationFiltration under suction

Sources & evidence

ORD record
ord-983482ff1c8c4987a8876f25444153da
Source dataset
uspto-grants-1976_03
Patent number
US03946032

Reaction notes

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