Hydrochloric Acid → 1-(4-Cyclopropanesulfonyl-2,3-difluoro-phenyl)-piperazine hydrochloride

HRID 1820812Notes

Reaction equation

C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([S:20]([CH:23]3[CH2:25][CH2:24]3)(=[O:22])=[O:21])=[C:16]([F:26])[C:15]=2[F:27])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:28]>O1CCOCC1>[ClH:28].[CH:23]1([S:20]([C:17]2[CH:18]=[CH:19][C:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)=[C:15]([F:27])[C:16]=2[F:26])(=[O:21])=[O:22])[CH2:25][CH2:24]1

Participants

Conditions

Temperature: 80 °C

Procedure

To 3.7 mmol 4-(4-Cyclopropanesulfonyl-2,3-difluoro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester in 100 ml dioxane was added 14.9 mmol HCl (as a 4 M solution in dioxane), and the mixture was heated at 80° C. for 1 h. The mixture was then cooled to room temperature, and the ensuing white crystals were collected by filtration, washing twice with ether, to afford the title compound. MS (m/e): 303.2 (M+H+, 100%)

Workup

temperatureThe mixture was then cooled to room temperature
filtrationthe ensuing white crystals were collected by filtration
washwashing twice with ether

Sources & evidence

ORD record: ord-dbe3e0449c724f48a9973cce7d4b8dad
Source dataset: uspto-grants-2009_10
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07605163B2

Reaction notes

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