Hydrogen chloride-ethyl acetate → HCID 178418230, compound

HRID 1351

Reaction equation

HRID 1351 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:14]=[CH:13][C:12]([C:15]([N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[C:21]3[NH:28][C:29]([CH3:31])=[N:30][C:20]=3[CH2:19][CH2:18]2)=[O:16])=[CH:11][CH:10]=1.[ClH:32].C(OCC)(=O)C>C(O)C>[ClH:32].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:10]=[CH:11][C:12]([C:15]([N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[C:21]3[NH:28][C:29]([CH3:31])=[N:30][C:20]=3[CH2:19][CH2:18]2)=[O:16])=[CH:13][CH:14]=1

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 178418428HCID 178418428, compound

Product 1

HCID 178418230HCID 178418230, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

6-[(2'-Methoxy-4-biphenylyl)carbonyl]-2-methyl-1,4,5,6-tetrahydroimidazo[4,5-d][1]benzazepine was dissolved in 4.8 ml of ethyl alcohol, the solution was mixed with 0.44 ml of 4N hydrochloric acid-ethyl acetate and cooled on an ice bath to effect crystal formation, and then the thus formed crystals were collected by filtration and washed with a small volume of ethyl alcohol to obtain 260 mg of 6-[(2'-methoxy-4-biphenylyl)carbonyl]-2-methyl-1,4,5,6-tetrahydroimidazo[4,5-d][1]benzazepine hydrochloride (Example 33(2)).

Workup

  1. temperaturecooled on an ice bath to effect crystal formation
  2. filtrationthe thus formed crystals were collected by filtration
  3. washwashed with a small volume of ethyl alcohol

Sources & evidence

ORD record
ord-8d43c74a9d90473996cdace2ba79d6f8
Source dataset
uspto-grants-1998_03
Patent number
US05723606

Linked notes

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