反応式
[CH3:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][NH:4][C@@H:3]1[CH2:8][N:9]1[C:17](=[O:18])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]1=[O:19].[F:20][C:21]1[C:22]([I:30])=[C:23]([CH:27]=[CH:28][CH:29]=1)[C:24](O)=[O:25].CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C(OCC)(=O)C>[F:20][C:21]1[C:22]([I:30])=[C:23]([CH:27]=[CH:28][CH:29]=1)[C:24]([N:4]1[CH2:5][CH2:6][CH2:7][C@@H:2]([CH3:1])[C@H:3]1[CH2:8][N:9]1[C:17](=[O:18])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]1=[O:19])=[O:25]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
A mixture of 2-(((2S,3R)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione (0.4 g, 1.55 mmol), 3-fluoro-2-iodobenzoic acid (0.37 g, 1.4 mmol), DIPEA (0.49 mL, 2.8 mmol) and HATU (0.53 g, 1.4 mmol) in DMF (10 mL) was stirred at rt for 1 h. The reaction mixture was diluted with ethyl acetate and washed with satd. aq. NaHCO3 and brine successively. The organic layer was separated, dried with MgSO4 and concentrated in vacuo. The crude product was purified by chromatography on silica gel (EtOAc/hex) to afford the title compound. MS (ESI) 507 (M+H).
後処理
- washwashed with satd
- customThe organic layer was separated
- dry with materialdried with MgSO4
- concentrationconcentrated in vacuo
- customThe crude product was purified by chromatography on silica gel (EtOAc/hex)
出典と根拠
- ORDレコード
- ord-371516814a414ec4a50a851945f310ce
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440982B2
関連ノート
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