反応式
O1CCCC1.O1CCCC1.C([N-]C(C)C)(C)C.[Li+].[C:19]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])(=[O:21])[CH3:20].[O:27]1[CH2:31][CH:30]=[CH:29][C:28]1=[O:32]>O>[C:23]([O:22][C:19](=[O:21])[CH2:20][CH:30]1[CH2:29][C:28](=[O:32])[O:27][CH2:31]1)([CH3:26])([CH3:25])[CH3:24]参加物
6
反応条件
- 温度
- -78 °C
実験手順
Tetrahydrofuran (50 mL) and Lithium diisopropylamide mono tetrahydrofuran complex (20 mL of 1.5 M in cyclohexane) was cooled in a dry ice/Isopropanol bath for 10 min. Tert-butyl acetate (3.5 mL 26 mmoles) was added via syringe and stirred at −78° C. for 30 min. 2(5H)-Furanone (1.59 g, 19 mmoles) was added dropwise and the reaction was stirred for 1 h at −78° C. The reaction was poured into water and extracted with ether 2×150 mL The ether extracts were combined and washed with water 100 mL then brine 3×100 mL, dried and the ether removed under reduced pressure to give 2.74 g of product (72%). MS (ESI+) for C10H16O4 m/z 223 (M+Na)+.
後処理
- stirringthe reaction was stirred for 1 h at −78° C
- extractionextracted with ether 2×150 mL The ether extracts
- washwashed with water 100 mL
- dry with materialbrine 3×100 mL, dried
- customthe ether removed under reduced pressure
出典と根拠
- ORDレコード
- ord-fc08a066caf44aa091c8db1dae39c476
- 出典データセット
- uspto-grants-2005_08
- 特許番号
- US06933304B2
関連ノート
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