Hydrochloric Acid → 1-(4-Cyclobutanesulfonyl-2-fluoro-phenyl)-piperazine hydrochloride

HRID 2251258노트

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HRID 2251258 반응식
[CH:1]1([S:5]([C:8]2[CH:13]=[CH:12][C:11](F)=[C:10]([F:15])[CH:9]=2)(=[O:7])=[O:6])[CH2:4][CH2:3][CH2:2]1.[NH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.[ClH:22]>CN(C)C(=O)C.O1CCOCC1>[ClH:22].[CH:1]1([S:5]([C:8]2[CH:13]=[CH:12][C:11]([N:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)=[C:10]([F:15])[CH:9]=2)(=[O:7])=[O:6])[CH2:4][CH2:3][CH2:2]1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 4837PiperazineHCID 69036720HCID 69036720, 화합물

생성물 1

HCID 690360641-(4-Cyclobutanesulfonyl-2-fluoro-phenyl)-piperazine hydrochloride

시약·촉매·용매 2

HCID 312751,4-Dioxane용매HCID 31374Dimethylacetamide용매

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온도
80 °C

실험 절차

To 2.8 mmol 4-cyclobutanesulfonyl-1,2-difluoro-benzene in 20 ml N,N-dimethylacetamide was added 8.3 mmol piperazine, and the mixture was heated at 80° C. for 45 min. The mixture was then concentrated in vacuo, and the residue was chromatographed on silica gel (eluant: ethyl acetate/methanol gradient). The product-containing fractions were combined and concentrated in vacuo. The residue was resuspended in 100 ml dioxane, and 6.0 mmol HCl (as a 4 M solution in dioxane) was added. After stirring for 10 min, the ensuing white crystals were collected by filtration, washing twice with ether, to afford the title compound.

후처리

  1. concentrationThe mixture was then concentrated in vacuo
  2. customthe residue was chromatographed on silica gel (eluant: ethyl acetate/methanol gradient)
  3. concentrationconcentrated in vacuo
  4. filtrationthe ensuing white crystals were collected by filtration
  5. washwashing twice with ether

출처 및 근거

ORD 기록
ord-60919453a5ea429fb90cd6db0dc80fb6
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07319099B2

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