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1-Methylpiperazine → 5-(4-Methylpiperazin-1-yl)-2-trifluoromethoxyphenylamine

HRID 1914758
ノート
印刷プレビュー

反応式

HRID 1914758 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]([O:9][C:10]([F:13])([F:12])[F:11])=[C:6]([NH2:8])[CH:7]=1.[Li]N([Si](C)(C)C)[Si](C)(C)C.[CH3:24][N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1>C1COCC1.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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2CCCCC2)C2C=CC=CC=2C2C=CC=CC=2N(C)C)CCCCC1>[CH3:24][N:25]1[CH2:30][CH2:29][N:28]([C:2]2[CH:3]=[CH:4][C:5]([O:9][C:10]([F:13])([F:12])[F:11])=[C:6]([NH2:8])[CH:7]=2)[CH2:27][CH2:26]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 531671-MethylpiperazineHCID 27793675-Bromo-2-(trifluoromethoxy)anilineHCID 178418261HCID 178418261、化合物

生成物 1

HCID 249941425-(4-Methylpiperazin-1-yl)-2-trifluoromethoxyphenylamine収率 64%

試薬・触媒・溶媒 3

HCID 27342172-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenyl触媒
HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 8028Tetrahydrofuran溶媒

実験手順

Tris(dibenzilideneacetone)dipalladium, Pd2(dba)3 (1.1 g, 1.2 mmol), 2-dicyclohexylphosphino-2′-(N,N-dimethylamino)-biphenyl (0.94 g, 2.4 mmol), 5-bromo-2-trifluoromethoxy-phenylamine (30.7 g, 120 mmol) in THF (50 mL) were charged in a round-bottom flask flushed with argon. The flask was evacuated and backfilled with argon. LiN(TMS)2 solution (1M in THF, 288 mL) and N-methylpiperazine (26.7 mL, 194 mmol) were added and the reaction refluxed for 1 h. The reaction mixture was then allowed to cool to room temperature and filtered through a pad of celite. The organic phase was concentrated, the residue dissolved in DCM (200 ml) and washed with water (1×100 ml). The organic phases were dried over anhydrous Na2SO4, the solvent evaporated in vacuo and the crude solid was purified by flash chromatography on silica gel (eluant: DCM/EtOH 90/10) to afford 21.1 g of 5-(4-methyl-piperazin-1-yl)-2-trifluoromethoxy-phenylamine (64% yield) as a light brown powder.

後処理

  1. customflushed with argon
  2. customThe flask was evacuated
  3. temperaturethe reaction refluxed for 1 h
  4. filtrationfiltered through a pad of celite
  5. concentrationThe organic phase was concentrated
  6. dissolutionthe residue dissolved in DCM (200 ml)
  7. washwashed with water (1×100 ml)
  8. dry with materialThe organic phases were dried over anhydrous Na2SO4
  9. customthe solvent evaporated in vacuo
  10. customthe crude solid was purified by flash chromatography on silica gel (eluant: DCM/EtOH 90/10)

出典と根拠

ORDレコード
ord-5c613f3e0c7c44888041ef8056620e2e
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08614220B2

反応ノート

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