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Tributylvinyltin → N-(2-benzoyl-4-vinylphenyl)-2,2,2-trifluoro-acetamide

HRID 2053424
ノート
印刷プレビュー

反応式

HRID 2053424 の反応式
[C:1]([C:9]1[CH:14]=[C:13](Br)[CH:12]=[CH:11][C:10]=1[NH:16][C:17](=[O:22])[C:18]([F:21])([F:20])[F:19])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:23]([Sn](CCCC)(CCCC)C=C)[CH2:24]CC>C1(C)C=CC=CC=1.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[C:1]([C:9]1[CH:14]=[C:13]([CH:23]=[CH2:24])[CH:12]=[CH:11][C:10]=1[NH:16][C:17](=[O:22])[C:18]([F:21])([F:20])[F:19])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 81998TributylvinyltinHCID 4702292N-(2-benzoyl-4-bromophenyl)-2,2,2-trifluoroacetamide

生成物 1

HCID 59655009N-(2-benzoyl-4-vinylphenyl)-2,2,2-trifluoro-acetamide収率 70%

試薬・触媒・溶媒 2

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒HCID 1140Toluene溶媒2 回

実験手順

To a solution of N-(2-benzoyl-4-bromophenyl)-2,2,2-trifluoroacetamide (a) (0.37 g, 1.0 mmol) in degassed dry toluene (10 mL) was added a solution of tetrakis(triphenyl-phosphine) palladium [Pd(PPh3)4] in toluene (5 mL) under argon. The mixture was heated to reflux and tributyl(vinyl)tin (0.29 mL, Immol) was added in a dropwise fashion. After refluxing overnight, the mixture was cooled to room temperature and filtered. The filtrate was concentrated and the residue was purified by flash chromatography on silica gel [hexanes: ethyl acetate (9:1)] to give N-(2-benzoyl-4-vinylphenyl)-2,2,2-trifluoro-acetamide (b) (0.22 g, 70%). 1H NMR (300 MHz, CDCl3) δ 12.0 (s, 1H), 8.62 (d, J=10.9 Hz, 1H), 7.80-7.60 (m, 5H), 7.60-7.43 (m, 2H), 6.65 (dd, J=11, 19.6 Hz, 1H), 5.69 (d, J=19.6 Hz, 1H), 5.29 (d, J=11 Hz,1H). MS: 320.2 (M+H).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureAfter refluxing overnight
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated
  6. customthe residue was purified by flash chromatography on silica gel [hexanes: ethyl acetate (9:1)]

出典と根拠

ORDレコード
ord-65932af4dbd54c528fb0a9285d7da086
出典データセット
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07326788B2

反応ノート

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