Ethyl Acetate → Methyl-3-oxo-6,8-dioxabicyclo[3.2.1]octane
反応式
C([O:8][CH2:9][CH:10]1[O:15][C:14](C)=[CH:13][C:12](=[O:17])[CH2:11]1)C1C=CC=CC=1.[CH3:18]COC(C)=O>[Pd]>[CH3:18][C:10]12[O:15][CH:14]([O:8][CH2:9]1)[CH2:13][C:12](=[O:17])[CH2:11]2参加物
4
実験手順
A solution of 4.4 g of the 6-Benzyloxy compound from Step 2 in EtOAc was hydrogenated with H2 and Pd/C (10%). After completion, the reaction was filtrated on a bed of celite and then evaporated to dryness. The cru syrup was then taken up in CH2Cl2 containing 1 g of camphor sulphonic acid. The reaction was stirred at r.t. overnight, filtered and evaporated. Purification by flash chromatography (30% Et2O/pentane) gave 780 mg of the title compound (30%).
後処理
- filtrationAfter completion, the reaction was filtrated on a bed of celite
- customevaporated to dryness
- filtrationfiltered
- customevaporated
- customPurification by flash chromatography (30% Et2O/pentane)
出典と根拠
- ORDレコード
- ord-eda2a644de254dfdb94eda29ec056675
- 出典データセット
- uspto-grants-1994_11
- 特許番号
- US05360815
反応ノート
読み込み中…