Piperazine → 1-[2-Fluoro-3-(methylthio)phenyl]piperazine

HRID 1879053

反応式

HRID 1879053 の反応式
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([S:8][CH3:9])[C:3]=1[F:10].[NH:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1.CC(C)([O-])C.[K+].P1(O)(OC2C=CC3C(C=2C2C4C(C=CC=2O1)=CC=CC=4)=CC=CC=3)=O>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].C1(C)C=CC=CC=1>[F:10][C:3]1[C:4]([S:8][CH3:9])=[CH:5][CH:6]=[CH:7][C:2]=1[N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1

参加物

7

反応物 4

HCID 4837PiperazineHCID 99589(+-)-1,1'-Binaphthyl-2,2'-diyl hydrogen phosphateHCID 23665647Potassium tert-butoxideHCID 574480643-Bromo-2-fluorothioanisole

生成物 1

HCID 574480731-[2-Fluoro-3-(methylthio)phenyl]piperazine

試薬・触媒・溶媒 2

HCID 6505921(1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium触媒HCID 1140Toluene溶媒

実験手順

Preparation according to preparation 22: 1-bromo-2-fluoro-3-(methylthio)benzene (2.15 g, 9.7 mmol), toluene (50 ml), piperazine (4.19 g, 48.5 mmol), potassium tert-butoxide (1.31 g, 13.6 mmol), bis(dibenzylideneacetone)palladium(0) (0.27 g, 0.064 mmol) and (+/−)-1,1′-binaphthyl-2,2′-diyl hydrogen phosphate (0.18 g, 0.064 mmol). Yield: 1.25 g. MS m/z (rel. intensity, 70 eV) 226 (M+, 20), 191 (12), 185 (10), 184 (bp), 168 (15).

後処理

  1. customPreparation
  2. customaccording to preparation 22

出典と根拠

ORDレコード
ord-c58db981c0bd4b369c6071f1da645b35
出典データセット
uspto-grants-2012_11
特許番号
US08314126B2

関連ノート

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