Dimethylamine → HCID 23328745, compound

HRID 225029Notes

Reaction equation

HRID 225029 reaction equation
Br[CH2:2][C:3]1[N:7]2[C:8]3[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:9]=3[C:10]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[N+:11]([O-:13])[CH2:12][C:6]2=[N:5][N:4]=1.[CH3:25][NH:26][CH3:27]>CN(C)C=O>[Cl:24][C:21]1[CH:22]=[CH:23][C:8]2[N:7]3[C:3]([CH2:2][N:26]([CH3:27])[CH3:25])=[N:4][N:5]=[C:6]3[CH2:12][N+:11]([O-:13])=[C:10]([C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:9]=2[CH:20]=1

Participants

4

Reactant 2

HCID 674DimethylamineHCID 23328735HCID 23328735, compound

Product 1

HCID 23328745HCID 23328745, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

To a suspension of 2.0 parts of 1-bromomethyl-8-chloro-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine 5-oxide in 20 volume parts of dimethylformamide is added 5 volume parts of 40 weight % aqueous solution of dimethylamine under stirring, and the resulting solution is stirred for 30 minutes at room temperature. After removing the solvent, the crystalline residue is recrystallized from ethyl alcohol to give 8-chloro-1-dimethylaminomethyl-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine 5-oxide as colorless prisms melting at 217° to 219° C.

Workup

  1. stirringthe resulting solution is stirred for 30 minutes at room temperature
  2. customAfter removing the solvent
  3. customthe crystalline residue is recrystallized from ethyl alcohol

Sources & evidence

ORD record
ord-a0513efaa395472b845f8576fec8b607
Source dataset
uspto-grants-1980_11
Patent number
US04235775

Reaction notes

Loading…