Hydrochloric Acid → HCID 67713711, compound

HRID 1378073Notes

Reaction equation

HRID 1378073 reaction equation
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15]4[N:19]=[C:18]([CH2:20][N:21]5[CH2:25][CH2:24][CH2:23][CH2:22]5)[O:17][N:16]=4)=[C:10]3[CH2:9][N:8]([CH3:26])[C:7](=[O:27])[C:6]=2[CH:28]=1.[ClH:29]>C(O)C>[ClH:29].[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][C:14]([C:15]4[N:19]=[C:18]([CH2:20][N:21]5[CH2:22][CH2:23][CH2:24][CH2:25]5)[O:17][N:16]=4)=[C:10]3[CH2:9][N:8]([CH3:26])[C:7](=[O:27])[C:6]=2[CH:28]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 22914635HCID 22914635, compound

Product 1

HCID 67713711HCID 67713711, compoundYield 96%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1.32, g (0.0035 mol) of 8-fluoro-5-methyl-3-(5-pyrrolidin-1-ylmethyl-1,2,4-oxadiazol-3-yl)-5,6-dihydro-4H-imidazo [1,5-a][1,4]benzodiazepin-6-one were dissolved in 50 ml of hot ethanol. 0.8 ml (0.0038 mol) of 4.78N ethanolic hydrochloric acid was added at room temperature. The solution was concentrated to a volume of ~20 ml, whereby crystallization began. 80 ml of ether were added, the mixture was filtered and there were obtained 1.38 g (96%) of 8-fluoro-5-methyl-3-(5-pyrrolidin-1-ylmethyl-1,2,4-oxadiazol-3-yl)-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodia-zepin-6-one hydrochloride (1:1) as white crystals; m.p. 243°-245° (dec.).

Workup

  1. concentrationThe solution was concentrated to a volume of ~20 ml, whereby crystallization
  2. addition80 ml of ether were added
  3. filtrationthe mixture was filtered

Sources & evidence

ORD record
ord-54e52f58800948c2ac395f358e8d9d9f
Source dataset
uspto-grants-1997_09
Patent number
US05665718

Reaction notes

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