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Piperidine → Tert-butyl(4-chloro-2-{[2-methyl-5-(propylsulfonyl)phenyl]ethynyl}phenoxy)acetate

HRID 2390137
ノート
印刷プレビュー

反応式

HRID 2390137 の反応式
Br[C:2]1[CH:7]=[C:6]([S:8]([CH2:11][CH2:12][CH3:13])(=[O:10])=[O:9])[CH:5]=[CH:4][C:3]=1[CH3:14].[C:15]([O:19][C:20](=[O:32])[CH2:21][O:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:24]=1[C:30]#[CH:31])([CH3:18])([CH3:17])[CH3:16].N1CCCCC1>CCOC(C)=O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[C:15]([O:19][C:20](=[O:32])[CH2:21][O:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:24]=1[C:30]#[C:31][C:2]1[CH:7]=[C:6]([S:8]([CH2:11][CH2:12][CH3:13])(=[O:10])=[O:9])[CH:5]=[CH:4][C:3]=1[CH3:14])([CH3:18])([CH3:17])[CH3:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8082PiperidineHCID 56594381Tert-butyl(4-chloro-2-ethynylphenoxy)acetate2 回HCID 585220912-Bromo-1-methyl-4-(propylsulfonyl)benzene2 回

生成物 1

HCID 58521875Tert-butyl(4-chloro-2-{[2-methyl-5-(propylsulfonyl)phenyl]ethynyl}phenoxy)acetate

試薬・触媒・溶媒 2

HCID 178418476HCID 178418476、化合物
触媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

A mixture of 2-bromo-1-methyl-4-(propylsulfonyl)benzene (Intermediate 37; 14.86 g, 53.6 mmol), tert-butyl(4-chloro-2-ethynylphenoxy)acetate (Intermediate 3, 13.00 g; 48.7 mmol), dichlorobis(triphenylphosphine)palladium(II) (1.37 g; 1.95 mmol) and piperidine (14.5 mL) was heated at 70° C. for 18 hours. The reaction mixture was taken up in EtOAc, washed twice with ammonium chloride and once with brine. The organic phase was dried over MgSO4, filtered and concentrated to dryness affording a crude, which was purified by flash column chromatography (silica), eluting with cyclohexane containing increasing amounts of EtOAc. The compound thus obtained as a brown sticky solid was recrystallized twice from EtOAc/petroleum ether to afford the title compound as a beige solid.

後処理

  1. washwashed twice with ammonium chloride and once with brine
  2. dry with materialThe organic phase was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated to dryness
  5. customaffording a crude, which
  6. customwas purified by flash column chromatography (silica)
  7. washeluting with cyclohexane containing
  8. temperatureincreasing amounts of EtOAc
  9. customThe compound thus obtained as a brown sticky solid
  10. customwas recrystallized twice from EtOAc/petroleum ether

出典と根拠

ORDレコード
ord-27458ffdb07e4658b50be3bec3f780e0
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273769B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート