1-(3-chloro-4-methylphenyl)ethanone → HCID 86631563、化合物

HRID 885815ノート

反応式

HRID 885815 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:10](=[O:15])[C:11]([F:14])([F:13])[F:12])[CH:5]=[C:6]([Br:9])[C:7]=1[F:8].[Cl:16][C:17]1[CH:18]=[C:19]([C:24](=[O:26])[CH3:25])[CH:20]=[CH:21][C:22]=1[CH3:23]>C(OCC)(=O)C>[Cl:16][C:17]1[CH:18]=[C:19]([C:24](=[O:26])[CH2:25][C:10]([C:4]2[CH:3]=[C:2]([Br:1])[C:7]([F:8])=[C:6]([Br:9])[CH:5]=2)([OH:15])[C:11]([F:14])([F:12])[F:13])[CH:20]=[CH:21][C:22]=1[CH3:23]

参加物

4

反応物 2

HCID 3429151-(3-chloro-4-methylphenyl)ethanoneHCID 86631564HCID 86631564、化合物

生成物 1

HCID 86631563HCID 86631563、化合物収率 95.4%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

To a stirred solution of 1-(3,5-dibromo-4-fluorophenyl)-2,2,2-trifluoroethanone (0.99 g) and 1-(3-chloro-4-methylphenyl)ethanone (0.48 g) in ethyl acetate (3 mL) was added dithylamine (0.062 g). The mixture was stirred at 50° C. for 2 hours. The reaction mixture was then concentrated under reduced pressure and the crude product was purified by liquid chromatography (medium pressure collection apparatus: Purif-α2 manufactured by Moritex Corporation) eluted with ethyl acetate-hexane (1:10) to afford the title compound as a pale yellow oil (1.40 g).

後処理

  1. concentrationThe reaction mixture was then concentrated under reduced pressure
  2. customthe crude product was purified by liquid chromatography (medium pressure collection apparatus: Purif-α2 manufactured by Moritex Corporation)
  3. washeluted with ethyl acetate-hexane (1:10)

出典と根拠

ORDレコード
ord-564f129e291d4d7a8f3c2e70671c819e
出典データセット
uspto-grants-2012_08
特許番号
US08242283B2

反応ノート

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