2-{(E)-2-[3-amino-5-(trifluoromethyl)phenyl]vinyl}-1H-isoindole-1,3(2H)-dione → Phthalimide
反応式
NC1C=C(/C=C/[N:14]2[C:22](=[O:23])[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15]2=[O:24])C=C(C(F)(F)F)C=1.[H][H]>[Pd].C1COCC1>[C:15]1(=[O:24])[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:22](=[O:23])[NH:14]1参加物
5
実験手順
A slurry of 2-{(E)-2-[3-amino-5-(trifluoromethyl)phenyl]vinyl}-1H-isoindole-1,3(2H)-dione (1.99 g, 5.98 nunol) and Pd/C (0.20 g, 10% by weight) in ETOH (123 mL) and THF (88 mL) was allowed to stir under 50 psi of hydrogen at rt until reaction was judged to be complete. The mixture was filtered through Celite and concentrated. The residue was purified by column chromatography to give 2-12-[3-amino-5-(trifluoromethyl)phenyl]ethyl)-1H-isoindole-1,3(2H)-dione (365 mg, 16% yield). LCMS: (FA) ES+ 335.
後処理
- filtrationThe mixture was filtered through Celite
- concentrationconcentrated
- customThe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-62e8a4d58e894cdfb2cb254d20db9221
- 出典データセット
- uspto-grants-2012_02
- 特許番号
- US08110687B2
反応ノート
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