Hydrochloric Acid → 1-[2-(Benzimidazol-2-ylthio)ethyl]piperazine

HRID 1350550Notes

Reaction equation

[N:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH:3][C:2]=1[S:10][CH2:11][CH2:12][N:13]1[CH2:18][CH2:17][N:16](C=O)[CH2:15][CH2:14]1.Cl.C(Cl)(Cl)Cl>CO>[N:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH:3][C:2]=1[S:10][CH2:11][CH2:12][N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1

Participants

Conditions

Temperature: 40 °C

Procedure

1-[2-(benzimidazol-2-ylthio)ethyl]-4-formylpiperazine (1.92 kg) was suspended in methanol (4.5 kg), and 12N hydrochloric acid (2.9 kg) was added, and the mixture was stirred at 40° C. for 3 hours. To the reaction solution was added chloroform (17 kg), and the precipitated crystals were collected by filtration. The crystals were washed with chloroform to give 2.38 kg of 1-[2-(benzimidazol-2-ylthio)ethyl]piperazine.3 hydrochloride (yield 97%) as colorless crystalline powder.

Workup

filtrationthe precipitated crystals were collected by filtration
washThe crystals were washed with chloroform

Sources & evidence

ORD record: ord-f83b8544d867473abb883e79f8bd0d5d
Source dataset: uspto-grants-2007_05
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07214796B2

Reaction notes

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