Hydrogen chloride-ethyl acetate → HCID 178418374, compound

HRID 1347

Reaction equation

HRID 1347 reaction equation
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:39]=[CH:38][CH:37]=[CH:36][C:9]=2[C:10]([NH:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]([N:21]3[C:27]4[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=4[C:25]4[NH:32][C:33]([CH3:35])=[N:34][C:24]=4[CH2:23][CH2:22]3)=[O:20])=[CH:15][CH:14]=2)=[O:11])=[CH:4][CH:3]=1.[ClH:40].C(OCC)(=O)C>C(O)C>[ClH:40].[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:39]=[CH:38][CH:37]=[CH:36][C:9]=2[C:10]([NH:12][C:13]2[CH:14]=[CH:15][C:16]([C:19]([N:21]3[C:27]4[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=4[C:25]4[NH:32][C:33]([CH3:35])=[N:34][C:24]=4[CH2:23][CH2:22]3)=[O:20])=[CH:17][CH:18]=2)=[O:11])=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 178418341HCID 178418341, compound

Product 1

HCID 178418374HCID 178418374, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

2-(4-Methylphenyl)-4'-[(2-methyl-1,4,5,6-tetrahydroimidazo[4,5-d][1]benzazepin-6-yl)carbonyl]benzanilide was dissolved in 10 ml of ethyl alcohol, the resulting solution was mixed with 0.37 ml of 4N hydrochloric acid-ethyl acetate and cooled on an ice bath and then the thus precipitated crystals were collected by filtration and washed with a small volume of ethyl alcohol to obtain 500 mg of 2-(4-methylphenyl)-4'-[(2-methyl-1,4,5,6-tetrahydroimidazo[4,5-d][1]benzazepin-6-yl)carbonyl]benzanilide hydrochloride (Example 19(2)).

Workup

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

Sources & evidence

ORD record
ord-58cd2e04d7a34df7b31f8a8ce82f18d5
Source dataset
uspto-grants-1998_03
Patent number
US05723606

Linked notes

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