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

HRID 2251258ノート

反応式

HRID 2251258 の反応式
[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

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 4837PiperazineHCID 69036720HCID 69036720、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 312751,4-Dioxane溶媒HCID 31374Dimethylacetamide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-60919453a5ea429fb90cd6db0dc80fb6
出典データセット
uspto-grants-2008_01
特許番号
US07319099B2

反応ノート

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