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Triethylamine → 2-{(E)-2-[3-amino-5-(trifluoromethyl)phenyl]vinyl}-1H-isoindole-1,3(2H)-dione

HRID 1640127
ノート
印刷プレビュー

反応式

HRID 1640127 の反応式
Br[C:2]1[CH:3]=[C:4]([CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1)[NH2:5].CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.CCN(CC)CC.[CH:42]([N:44]1[C:52](=[O:53])[C:51]2[C:46](=[CH:47][CH:48]=[CH:49][CH:50]=2)[C:45]1=[O:54])=[CH2:43]>C(C#N)(C)=O.CC([O-])=O.CC([O-])=O.[Pd+2]>[NH2:5][C:4]1[CH:3]=[C:2](/[CH:43]=[CH:42]/[N:44]2[C:45](=[O:54])[C:46]3[C:51](=[CH:50][CH:49]=[CH:48][CH:47]=3)[C:52]2=[O:53])[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 770351H-Isoindole-1,3(2H)-dione, 2-ethenyl-HCID 80271Tri-o-tolylphosphineHCID 27358803-Bromo-5-(trifluoromethyl)aniline

生成物 1

HCID 591349702-{(E)-2-[3-amino-5-(trifluoromethyl)phenyl]vinyl}-1H-isoindole-1,3(2H)-dione収率 28.8%

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
HCID 694302-Oxopropiononitrile溶媒

実験手順

3-Bromo-5-(trifluoromethyl)aniline (5.00 g, 0.0208 mol) was dissolved in AcCN (200 mL) and the solution was degassed with N2. Pd(OAc)2 (230 mg, 1.02 mmol), tris(2-methylphenyl)phosphine (630 mg, 2.07 mmol), and Et3N (5.75 mL, 0.041 mol) were added and the bright orange solution was allowed to stir at rt for 1 h. To this solution was added 2-vinyl-1H-isoindole-1,3(2H)-dione (3.61 g, 0.021 mol) and the reaction mixture was degassed and heated at reflux for 16 h. The reaction was filtered through Celite. The filtrate was washed with water and brine, dried over Na2SO4, filtered and concentrated. The residue was purified by column chromatography to give 2-{(E)-2-[3-amino-5-(trifluoromethyl)phenyl]vinyl}-1H-isoindole-1,3(2H)-dione (1.99 g, 24% yield). LCMS: (FA) ES+ 334.

後処理

  1. customthe solution was degassed with N2
  2. customthe reaction mixture was degassed
  3. temperatureheated
  4. temperatureat reflux for 16 h
  5. filtrationThe reaction was filtered through Celite
  6. washThe filtrate was washed with water and brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-79106a2bcccd4829a711477cc07df78d
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08110687B2

反応ノート

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