Dimethylamine → HCID 12404529, compound

HRID 2399148Notes

Reaction equation

HRID 2399148 reaction equation
[CH3:1][NH:2][CH3:3].CN.C([O:8][C:9]([C:11]1[N:32]=[C:14]2[CH2:15][N:16]=[C:17]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=3[F:31])[C:18]3[CH:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:19]=3[N:13]2[N:12]=1)=O)C>CO>[CH3:1][N:2]([CH3:3])[C:9]([C:11]1[N:32]=[C:14]2[CH2:15][N:16]=[C:17]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=3[F:31])[C:18]3[CH:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:19]=3[N:13]2[N:12]=1)=[O:8]

Participants

5

Reactant 3

HCID 674DimethylamineHCID 6329MethylamineHCID 57147673HCID 57147673, compound

Product 1

HCID 12404529HCID 12404529, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Pure gaseous dimethylamine free, in particular, from methylamine, is fed for two hours at room temperature, with stirring, into a suspension of 3.85 (0.01 mole) of 6-(o-fluorophenyl)-8-chloro-4H-s-triazolo[1,5-a][1,4]benzodiazepine-2-carboxylic acid ethyl ester [cp. Example 2(a)- (c)] in 200 ml of methanol. The clear reaction mixture is concentrated in vacuo to dryness. After recrystallisation from isopropanol, the residue yields pure N,N-dimethyl-6-(o-fluorophenyl)-8-chloro-4H-s-triazolo[1,5-a][1,4]benzodiazepine-2-carboxamide, M.P. 180°-182°.

Workup

  1. concentrationThe clear reaction mixture is concentrated in vacuo to dryness
  2. customAfter recrystallisation from isopropanol

Sources & evidence

ORD record
ord-92fb9a2cdaba4156a04b9964c6c269e4
Source dataset
uspto-grants-1977_05
Patent number
US04027029

Reaction notes

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