Hydrochloric Acid → 1-[2,3-Difluoro-4-(propane-2-sulfonyl)-phenyl]-piperazine hydrochloride

HRID 2251263Notes

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]([CH3:25])[CH3:24])(=[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].[F:27][C:15]1[C:16]([F:26])=[C:17]([S:20]([CH:23]([CH3:25])[CH3:24])(=[O:21])=[O:22])[CH:18]=[CH:19][C:14]=1[N:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1

Participants

Conditions

Temperature: 80 °C

Procedure

To 7.5 mmol 4-[2,3-difluoro-4-(propane-2-sulfonyl)-phenyl]-piperazine-1-carboxylic acid tert-butyl ester in 100 ml dioxane was added 30.2 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.

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-5503e18cf9434df8850e8abb29fbb99b
Source dataset: uspto-grants-2008_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07319099B2

Reaction notes

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