反応式
[C:1]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.S(=O)(=O)(O)O.[C:14](OCC)(=[O:16])C.CCCCCC>CO>[OH:16][CH2:14][CH2:5][CH2:4][CH2:3][CH2:2][C:1]([O:7][CH3:6])=[O:8]参加物
5
実験手順
ε-Caprolactone (12.50 g, 109.51 mM) was dissolved in methanol (125 ml), and a sulfuric acid solution (1 ml, 0.01 mM) was slowly added thereto. The resulting mixture was stirred at room temperature for 2 days. After the completion of reaction, methanol was removed under reduced pressure, and then ice water was poured into the residue. The resulting mixture was extracted with ethyl ether. The organic layer was separated, washed with an aqueous saturated sodium bicarbonate solution and brine in order and concentrated under reduced pressure. The residue thus obtained was subjected to a silica gel column chromatography (eluent: ethyl acetate/n-hexane=1/2) to obtain 10.18 g of the title compound (yield 64%).
後処理
- customwas removed under reduced pressure
- additionice water was poured into the residue
- extractionThe resulting mixture was extracted with ethyl ether
- customThe organic layer was separated
- washwashed with an aqueous saturated sodium bicarbonate solution and brine in order
- concentrationconcentrated under reduced pressure
- customThe residue thus obtained
出典と根拠
- ORDレコード
- ord-86c877d7167f4648941ef009bc81d594
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08053435B2
関連ノート
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