tert-Butyl (S)-2-(2,2-dimethyl-4,6-dioxo-1,3-dioxane-5-carbonyl)pyrrolidine-1-carboxylate → Tert-butyl (3-oxopropanoyl)-1-pyrrolidinecarboxylate
反応式
CC1(C)OC(=O)[CH:5]([C:9]([C@@H:11]2[CH2:15][CH2:14][CH2:13][N:12]2[C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])=[O:10])[C:4](=O)[O:3]1>C1(C)C=CC=CC=1>[O:3]=[CH:4][CH2:5][C:9]([CH:11]1[CH2:15][CH2:14][CH2:13][N:12]1[C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])=[O:10]参加物
3
反応条件
- 温度
- 80 °C
実験手順
ArgoGel-OH (45 g, 0.49 meq/g, 22 mmol) was suspended in toluene (400 mL) and tert-butyl (2S)-2-[(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-yl)carbonyl]-1-pyrrolidinecarboxylate (60. g, 176 mmol) was added. The sealed reaction tube was heated at 80° C. for 23 h. The reaction mixture was allowed to cool to room temperature and filtered. The resin was washed (DMF then DCM then ether; 8× each) then dried at 40° C. overnight under high vacuum (63 g; 0.44 meq/g).
後処理
- customThe sealed reaction tube
- temperatureto cool to room temperature
- filtrationfiltered
- washThe resin was washed (DMF
- custom8× each) then dried at 40° C. overnight under high vacuum (63 g; 0.44 meq/g)
出典と根拠
- ORDレコード
- ord-90a804577e34449da10d0f04fe6b99e1
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07189851B2
反応ノート
読み込み中…