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Ethyl Acetate → HCID 18476298、化合物

HRID 2187658
ノート
印刷プレビュー

反応式

HRID 2187658 の反応式
[F:1][C:2]([F:12])([F:11])[O:3][C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[CH:6][CH:5]=1.[CH3:13][C:14]1[CH:23]=[CH:22][C:17]([C:18](=O)[CH2:19]Br)=[CH:16][CH:15]=1.C(OCC)(=O)C>C(N(CC)C1C=CC=CC=1)C.C1(C)C(C)=CC=CC=1>[CH3:13][C:14]1[CH:23]=[CH:22][C:17]([C:18]2[NH:8][C:7]3[C:9]([CH:19]=2)=[CH:10][C:4]([O:3][C:2]([F:11])([F:12])[F:1])=[CH:5][CH:6]=3)=[CH:16][CH:15]=1
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 8857Ethyl AcetateHCID 692722-Bromo-4'-methylacetophenoneHCID 6008484-(Trifluoromethoxy)aniline

生成物 1

HCID 18476298HCID 18476298、化合物

試薬・触媒・溶媒 2

HCID 7061N,N-Diethylaniline溶媒HCID 7237O-Xylene溶媒

反応条件

温度
165 °C

実験手順

To a stirred solution of 5.3 g (30 mmol) of 4-trifluoromethoxyaniline in 8 ml of N,N-diethylaniline was added dropwise at 165° C. a solution of 4.3 g of 4-methylphenacyl bromide in 7.5 ml of xylene. It was heated at 165° C. for 3 h. The mixture was cooled followed by addition of 50 ml of ethyl acetate. It was washed with 2N hydrochloric acid, and the aqueous layer was extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure. The residue was purified via repeated column chromatography on silica gel using a hexane dichloromethane gradient (100:0 to 50:50). The title compound thus obtained was recrystallized from hexane.

後処理

  1. temperatureThe mixture was cooled
  2. washIt was washed with 2N hydrochloric acid
  3. extractionthe aqueous layer was extracted with ethyl acetate
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified

出典と根拠

ORDレコード
ord-eede3d8a353b4546b4af70361fda20d9
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06410562B1

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