Hydrochloric Acid → HCID 21842228, compound

HRID 1418896Notes

Reaction equation

HRID 1418896 reaction equation
[CH2:1]([N:4]([CH2:8][C:9]1[O:13][C:12]([C:14]2[N:15]=[CH:16][N:17]3[C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=4[C:21](=[O:28])[N:20]([CH3:29])[CH2:19][C:18]=23)=[N:11][CH:10]=1)[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3].[ClH:30]>C(OCC)(=O)C>[ClH:30].[CH2:1]([N:4]([CH2:8][C:9]1[O:13][C:12]([C:14]2[N:15]=[CH:16][N:17]3[C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=4[C:21](=[O:28])[N:20]([CH3:29])[CH2:19][C:18]=23)=[N:11][CH:10]=1)[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21842229HCID 21842229, compound

Product 1

HCID 21842228HCID 21842228, compoundYield 87%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

1.0 g (0.00254 mol) of 3-(5-dipropylaminomethyl-oxazol-2-yl)-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one in 50 ml of ethyl acetate was treated with 0.76 ml (0.00279 mol) of 3.7N ethanolic hydrochloric acid. After stirring at 0° for 1/2 hr. the white suspension was suction filtered. The yellowish crystals were dissolved in hot acetonitrile and recrystallized by the addition of ether. There was obtained 0.95 g (87%) of 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 light beige crystals; m.p. 228°-231° (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-5c1d3be54eb14307ae6c333aaf53872f
Source dataset
uspto-grants-1999_03
Patent number
US05885986

Reaction notes

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