反応式
[CH3:1][C:2]1([OH:12])[CH2:11][CH2:10][C:5]2(OCC[O:6]2)[CH2:4][CH2:3]1.Cl>C1COCC1>[OH:12][C:2]1([CH3:1])[CH2:11][CH2:10][C:5](=[O:6])[CH2:4][CH2:3]1参加物
4
実験手順
8-Methyl-1,4-dioxaspiro[4.5]decane-8-ol (650 mg, 3.77 mmol) was dissolved in THF (10 ml), followed by addition of 1N aqueous HCl solution (5 ml), and then the resulting mixture was stirred at room temperature for 6 hours. The resulting reaction liquid was concentrated under reduced pressure, and then extracted with 10% MeOH/MC (20 ml×5). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (50% EtOAc/Hexanes), to obtain 443 mg of yellow oil (92%).
後処理
- customThe resulting reaction liquid
- concentrationwas concentrated under reduced pressure
- extractionextracted with 10% MeOH/MC (20 ml×5)
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfollowed by filtration and concentration
- customthe residue thus obtained
出典と根拠
- ORDレコード
- ord-4c8d104f2237465ead45294b8349f757
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096571B2
関連ノート
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