反応式
[O:1]=[C:2]([CH2:9][CH2:10][CH3:11])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[CH2:12](O)[CH2:13][CH2:14][OH:15].C(OC)(OC)OC.C(N(CC)CC)C>O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH2:7]([O:6][C:4](=[O:5])[CH2:3][C:2]1([CH2:9][CH2:10][CH3:11])[O:15][CH2:14][CH2:13][CH2:12][O:1]1)[CH3:8]参加物
6
実験手順
A mixture of ethyl 3-oxohexanoate (5 g, 31.6 mmol), 1,3-propanediol (3.61 g, 47.4 mmol), trimethyl orthoformate (5.78 ml, 34.8 mmol), and p-toluenesulfonic acid monohydrate (272 mg, 1.58 mmol) was stirred at room temperature for 22 hours. After completion of the reaction, triethylamine (881 μl, 6.32 mmol) was added to the reaction mixture which was then concentrated. The residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate) to obtain the title compound (5.5 g, yield: 80.5%) as a light yellow oil.
後処理
- additionwas added to the reaction mixture which
- concentrationwas then concentrated
- customThe residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate)
出典と根拠
- ORDレコード
- ord-53ba594080f34bdaace61d7e57e41a9f
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07425634B2
関連ノート
読み込み中…