反応式
[OH:1][C:2]1[CH:3]=[C:4]([C:12]([O:14][CH3:15])=[O:13])[CH:5]=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].CS(O[CH2:21][CH2:22][CH2:23][N:24]([C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])[CH2:25][CH:26]([CH3:28])[CH3:27])(=O)=O>CC#N>[C:32]([O:31][C:29]([N:24]([CH2:25][CH:26]([CH3:27])[CH3:28])[CH2:23][CH2:22][CH2:21][O:1][C:2]1[CH:11]=[C:6]([C:7]([O:9][CH3:10])=[O:8])[CH:5]=[C:4]([CH:3]=1)[C:12]([O:14][CH3:15])=[O:13])=[O:30])([CH3:34])([CH3:35])[CH3:33]参加物
4
実験手順
Dimethyl 5-hydroxyisophthalate (0.30 g, 1.44 mmol) cesium carbonate (0.95 g, 2.88 mmol) and CH3CN (25 mL) were stirred for 30 min. 3-((tert-Butoxycarbonyl)(isobutyl)amino)-propyl methanesulfonate (0.63 g, 2.02 mmol) was added, and the reaction mixture was stirred for 16 h. The reaction mixture was concentrated under reduced pressure and partitioned between EtOAc (50 mL) and H2O (50 mL). The layers were separated, and the aqueous layer was extracted with EtOAc (50 mL). The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure to afford the desired product, which was used without further purification.
後処理
- concentrationThe reaction mixture was concentrated under reduced pressure
- custompartitioned between EtOAc (50 mL) and H2O (50 mL)
- customThe layers were separated
- extractionthe aqueous layer was extracted with EtOAc (50 mL)
- dry with materialThe combined organics were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-af1d9475293f4e76a9fa8e3869faf4a5
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09439433B2
関連ノート
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