Pyridine → HCID 86638587、化合物

HRID 1807810ノート

反応式

HRID 1807810 の反応式
[F:1][C:2]([F:23])([F:22])[C:3]([C:9]1[CH:14]=[CH:13][C:12]([CH2:15][N:16]2[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]2)=[CH:11][CH:10]=1)([OH:8])[C:4]([F:7])([F:6])[F:5].[N+:24]([C:27]1[CH:28]=[C:29]([S:33](Cl)(=[O:35])=[O:34])[CH:30]=[CH:31][CH:32]=1)([O-:26])=[O:25].N1C=CC=CC=1>ClCCl>[F:23][C:2]([F:22])([F:1])[C:3]([C:9]1[CH:10]=[CH:11][C:12]([CH2:15][N:16]2[CH2:17][CH2:18][N:19]([S:33]([C:29]3[CH:30]=[CH:31][CH:32]=[C:27]([N+:24]([O-:26])=[O:25])[CH:28]=3)(=[O:34])=[O:35])[CH2:20][CH2:21]2)=[CH:13][CH:14]=1)([OH:8])[C:4]([F:7])([F:6])[F:5]

参加物

5

反応物 3

HCID 1049PyridineHCID 84763-Nitrobenzenesulfonyl chlorideHCID 866385661,1,1,3,3,3-Hexafluoro-2-(4-(piperazin-1-ylmethyl)phenyl)propan-2-ol

生成物 1

HCID 86638587HCID 86638587、化合物収率 70.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1,1,1,3,3,3-Hexafluoro-2-(4-(piperazin-1-ylmethyl)phenyl)propan-2-ol (2.366 mmol, 810 mg), 3-nitrobenzene-1-sulfonyl chloride (2.366 mmol, 524 mg) and pyridine (4.73 mmol, 0.383 mL, 374 mg) were combined in dichloromethane (20 mL) and stirred at room temperature for 1 hour. The reaction mixture was washed with water, and the organic layer was separated, dried and concentrated under vacuum. The residue was purified by SCX chromatography to afford the title compound (875.3 mg). MS (ESI) m/z 528.0 [M+H]+

後処理

  1. washThe reaction mixture was washed with water
  2. customthe organic layer was separated
  3. customdried
  4. concentrationconcentrated under vacuum
  5. customThe residue was purified by SCX chromatography

出典と根拠

ORDレコード
ord-e5e66da1e1274f31a572868af1fd973b
出典データセット
uspto-grants-2013_01
特許番号
US08357679B2

反応ノート

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