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HCID 67207151、化合物 → HCID 58288421、化合物

HRID 1476094
ノート
印刷プレビュー

反応式

HRID 1476094 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]([C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([N+:17]([O-])=O)[CH:11]=1)=[CH:4][C:5]([O:7][CH2:8][CH3:9])=[O:6]>C(O)C.[Pd]>[NH2:17][C:12]1[CH:11]=[C:10]([CH:3]([C:2]([F:21])([F:1])[F:20])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH:15]=[CH:14][C:13]=1[F:16]
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 1

HCID 67207151HCID 67207151、化合物

生成物 1

HCID 58288421HCID 58288421、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

5.0 g (16.3 mmol) of ethyl 4,4,4-trifluoro-3-(4-fluoro-3-nitrophenyl)but-2-enoate were dissolved in 133 ml of ethanol, and 866 mg of palladium on carbon (10%) were added under argon. At RT, the reaction mixture was stirred vigorously under an atmosphere of hydrogen (atmospheric pressure) overnight. The mixture was then filtered off through celite and the residue was washed with ethyl acetate. The filtrate was concentrated under reduced pressure and the residue obtained was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 50:1). This gave 3.91 g of the target product (85.9% of theory).

後処理

  1. filtrationThe mixture was then filtered off through celite
  2. washthe residue was washed with ethyl acetate
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe residue obtained
  5. customwas purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 50:1)

出典と根拠

ORDレコード
ord-49245502d661459bbc5a70822d3bdc9e
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018414B2

反応ノート

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