Triethylamine → N-(1-(2-bromo-4-chlorophenyl)ethyl)-4'-fluoro-[1,1'-biphenyl]-4-amine

HRID 405235ノート

反応式

HRID 405235 の反応式
CS(Cl)(=O)=O.[Br:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[CH:14](O)[CH3:15].CCN(CC)CC.[F:24][C:25]1[CH:30]=[CH:29][C:28]([C:31]2[CH:36]=[CH:35][C:34]([NH2:37])=[CH:33][CH:32]=2)=[CH:27][CH:26]=1>C(Cl)Cl>[Br:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[CH:14]([NH:37][C:34]1[CH:33]=[CH:32][C:31]([C:28]2[CH:29]=[CH:30][C:25]([F:24])=[CH:26][CH:27]=2)=[CH:36][CH:35]=1)[CH3:15]

参加物

6

反応物 4

HCID 8471Triethylamine2 回HCID 94624'-Fluoro(1,1'-biphenyl)-4-amineHCID 31297Methanesulfonyl chlorideHCID 574450731-(2-Bromo-4-chlorophenyl)ethanol

生成物 1

HCID 71060075N-(1-(2-bromo-4-chlorophenyl)ethyl)-4'-fluoro-[1,1'-biphenyl]-4-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Neat methanesulfonyl chloride (0.18 mL, 2.4 mmol) was added to a 0° C., DCM solution (20 mL) of 1-(2-bromo-4-chlorophenyl)ethanol (558 mg, 2.4 mmol) and Et3N (0.36 mL, 2.6 mmol) and the resulting mixture was allowed to warm to room temperature gradually. After 30 min Et3N (0.36 mL, 2.6 mmol) and 4′-fluoro-[1,1′-biphenyl]-4-amine (444 g, 2.4 mmol) were added sequentially and stirred at room temperature. After 16 h the resulting mixture was concentrated and purified via column chromatography to yield the title compound.

後処理

  1. concentrationAfter 16 h the resulting mixture was concentrated
  2. custompurified via column chromatography

出典と根拠

ORDレコード
ord-caeff1b21d554846b9dfa00a271a2c41
出典データセット
uspto-grants-2014_06
特許番号
US08748624B2

反応ノート

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