Hydrogen chloride-ethyl acetate → HCID 22013777, compound

HRID 1532692Notes

Reaction equation

HRID 1532692 reaction equation
[ClH:1].C(OCC)(=O)C.[CH3:8][N:9]([CH3:42])[CH2:10][CH2:11][N:12]1[C:16]2[CH:17]=[CH:18][C:19]([C:21]([NH:23][CH3:24])=[O:22])=[CH:20][C:15]=2[N:14]=[C:13]1[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41]>C(OCC)(=O)C.C(O)C>[ClH:1].[CH3:8][N:9]([CH3:42])[CH2:10][CH2:11][N:12]1[C:16]2[CH:17]=[CH:18][C:19]([C:21]([NH:23][CH3:24])=[O:22])=[CH:20][C:15]=2[N:14]=[C:13]1[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41]

Participants

5

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 22013765HCID 22013765, compound

Product 1

HCID 22013777HCID 22013777, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

4N Hydrochloric acid/ethyl acetate solution (1.24 ml) was added to a solution containing 1-[2-(dimethylamino)ethyl]-2-heptadecyl-N-methyl-1H-benzimidazole-5-carboxamide (2.207 g) in a mixture of ethyl acetate (22 ml) and ethanol (2 ml). After being stirred for 30 minutes while being cooled with ice, the reaction mixture was concentrated. The residue was recrystallized with the mixed solution of ethyl acetate-ethanol, thereby yielding the entitled compound (1.751 g) as white crystals.

Workup

  1. temperaturewhile being cooled with ice
  2. concentrationthe reaction mixture was concentrated
  3. customThe residue was recrystallized with the mixed solution of ethyl acetate-ethanol

Sources & evidence

ORD record
ord-fe0ea16a2d7a42b3ba1d89e5c62176fb
Source dataset
uspto-grants-2001_03
Patent number
US06204264B1

Reaction notes

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