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2,2,2-Trifluoroethanesulfonyl chloride → N-[2-({3-Chloro-4-[(2-methylphenyl)carbonyl]phenyl}amino)benzyl]-2,2,2-trifluoroethanesulfonamide

HRID 1797311
ノート
印刷プレビュー

反応式

HRID 1797311 の反応式
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[CH3:24])=[O:17])=[C:12]([Cl:25])[CH:11]=1.[F:26][C:27]([F:34])([F:33])[CH2:28][S:29](Cl)(=[O:31])=[O:30]>N1C=CC=CC=1>[Cl:25][C:12]1[CH:11]=[C:10]([NH:9][C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[CH2:2][NH:1][S:29]([CH2:28][C:27]([F:34])([F:33])[F:26])(=[O:31])=[O:30])[CH:15]=[CH:14][C:13]=1[C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[CH3:24])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 742422,2,2-Trifluoroethanesulfonyl chlorideHCID 22174531(4-{[2-(Aminomethyl)phenyl]amino}-2-chlorophenyl)(2-methylphenyl)methanone

生成物 1

HCID 22174499N-[2-({3-Chloro-4-[(2-methylphenyl)carbonyl]phenyl}amino)benzyl]-2,2,2-trifluoroethanesulfonamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Compound 148 (0.18 g, 0.71 mmol) was dissolved in dry pyridine (0.9 mL) and 2,2,2-trifluoroethanesulfonyl chloride (0.12 mL, 1.1 mmol) was added. The solution was stirred at room temperature for 1 h after which it was concentrated in vacuo. The oil was diluted with H2O and the water phase was extracted three times with EtOAc. The combined organic phases were washed with 10% aqueous NaHCO3, dried (MgSO4), filtered and concentrated in vacuo. The crude product was purified by flash chromatography using EtOAc/petroleum ether 1:2 as the eluent to afford the title compound as a yellow oil.

後処理

  1. concentrationwas concentrated in vacuo
  2. additionThe oil was diluted with H2O
  3. extractionthe water phase was extracted three times with EtOAc
  4. washThe combined organic phases were washed with 10% aqueous NaHCO3
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe crude product was purified by flash chromatography

出典と根拠

ORDレコード
ord-e5d7ff4b78074324995318fec3a48543
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07034015B2

反応ノート

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