Hydrochloric Acid → HCID 21842274, compound

HRID 1418900Notes

Reaction equation

HRID 1418900 reaction equation
[Cl:1][C:2]1[C:7]2[C:8](=[O:30])[N:9]([CH3:29])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[O:17][C:18]([CH2:21][N:22]([CH2:26][CH2:27][CH3:28])[CH2:23][CH2:24][CH3:25])=[CH:19][N:20]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1.Cl>C(OCC)(=O)C>[ClH:1].[Cl:1][C:2]1[C:7]2[C:8](=[O:30])[N:9]([CH3:29])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[O:17][C:18]([CH2:21][N:22]([CH2:26][CH2:27][CH3:28])[CH2:23][CH2:24][CH3:25])=[CH:19][N:20]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21842252HCID 21842252, compound

Product 1

HCID 21842274HCID 21842274, compoundYield 158.4%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

1.2 g (0.0028 mol) of 7-chloro-3-(5-dipropylaminomethyloxazol-2-yl)-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]-benzodiazepin-6-one in 80 ml of ethyl acetate were treated at 0° with 0.84 ml (0.0031 mol) of 3.7N ethanolic hydrochloric acid. After stirring at 0° for 15 minutes the white suspension was suction filtered. The yellowish crystals were dissolved in hot acetonitrile and recrystallized by the addition of ether. There were obtained 1.03 g (79%) of 7-chloro-3-(5-dipropylaminomethyl-oxazol-2-yl)-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one hydrochloride (1:1) as white crystals; m.p. 218°-210° (dec.).

Workup

  1. filtrationsuction filtered
  2. dissolutionThe yellowish crystals were dissolved in hot acetonitrile
  3. customrecrystallized by the addition of ether

Sources & evidence

ORD record
ord-2116ffe490ae40c990202172654dd19a
Source dataset
uspto-grants-1999_03
Patent number
US05885986

Reaction notes

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