Ethanol → 4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl) [1,4]diazepane hydriodic acid salt

HRID 2230499Notes

Reaction equation

HRID 2230499 reaction equation
[CH2:1]([O:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]=[C:7]1[N:15]1[CH2:21][CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)[CH3:2].[IH:22].C(O)C>C(OCC)C>[IH:22].[CH2:1]([O:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]=[C:7]1[N:15]1[CH2:21][CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)[CH3:2]

Participants

5

Reactant 3

HCID 702EthanolHCID 24841Hydrogen iodideHCID 9984168Emedastine EP Impurity E

Product 1

HCID 865838874-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl) [1,4]diazepane hydriodic acid salt

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

Combine 4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (1.30 g), 48% hydriodic acid (10 mL), ethanol (10 mL), and diethyl ether (80 mL) and stir. After 30 minutes add diethyl ether, (800 mL) and continue to stir to give a solid. Collect the solid by filtration and dry in vacuo to give the title compound: mp; 156-163° C.

Workup

  1. customto give a solid
  2. customCollect the solid
  3. filtrationby filtration
  4. customdry in vacuo

Sources & evidence

ORD record
ord-6d692df9f44247cbb6784a97228102f1
Source dataset
uspto-grants-2002_07
Patent number
US06423704B1

Reaction notes

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