7-(4-dimethylaminophenyl)-N-(4-((1-oxophosphorinan-1-yl)methyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide → 7-(4-dimethylaminophenyl)-N-(4-((1-oxophosphorinan-1-yl)methyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide hydrochloride

HRID 2228144Notes

Reaction equation

HRID 2228144 reaction equation
[CH3:1][N:2]([CH3:37])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[O:18][CH2:17][CH2:16][C:15]([C:19]([NH:21][C:22]4[CH:27]=[CH:26][C:25]([CH2:28][P:29]5(=[O:35])[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]5)=[CH:24][CH:23]=4)=[O:20])=[CH:14][C:13]=3[CH:36]=2)=[CH:5][CH:4]=1.[ClH:38].C(OCC)(=O)C>C(O)C>[ClH:38].[CH3:1][N:2]([CH3:37])[C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[O:18][CH2:17][CH2:16][C:15]([C:19]([NH:21][C:22]4[CH:27]=[CH:26][C:25]([CH2:28][P:29]5(=[O:35])[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]5)=[CH:24][CH:23]=4)=[O:20])=[CH:14][C:13]=3[CH:36]=2)=[CH:7][CH:8]=1

Participants

4

Reactant 2

HCID 184722457-(4-dimethylaminophenyl)-N-(4-((1-oxophosphorinan-1-yl)methyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamideHCID 21866389Hydrogen chloride-ethyl acetate

Product 1

HCID 184722807-(4-dimethylaminophenyl)-N-(4-((1-oxophosphorinan-1-yl)methyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide hydrochloride

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 7—(4-dimethylaminophenyl)-N-(4—((1-oxophosphorinan-1-yl)methyl)phenyl)-2.3-dihydro-1-benzoxepine-4-carboxamide (0.1 g) in ethanol was added 4N hydrochloric acid-ethyl acetate (0.2 ml) under ice-cooling. The solvent was evaporated, and the residue was crystallized from ethanol and diethylether to give 7—(4-dimethylaminophenyl)-N-(4—((1-oxophosphorinan-1-yl)methyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide hydrochloride (Compound 155) (0.1 g) as colorless crystals.

Workup

  1. temperaturecooling
  2. customThe solvent was evaporated
  3. customthe residue was crystallized from ethanol and diethylether

Sources & evidence

ORD record
ord-cb780e0684884166a0bc2988bdb5b748
Source dataset
uspto-grants-2002_07
Patent number
US06413947B1

Reaction notes

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