Trimethyl orthoformate → (2-Methoxy-1,3-dioxan-5-yl)methanol
反応式
[OH:1][CH2:2][CH:3]([CH2:6][OH:7])[CH2:4][OH:5].[CH:8](OC)(OC)[O:9][CH3:10].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(N(CC)CC)C>[CH3:8][O:9][CH:10]1[O:5][CH2:4][CH:3]([CH2:6][OH:7])[CH2:2][O:1]1参加物
5
実験手順
A mixture of 2-(hydroxymethyl)-1,3-propanediol (1.7 g, 16 mmol), trimethyl orthoformate (7 ml, 64.1 mmol), and p-toluenesulfonic acid monohydrate (275 mg, 1.6 mmol) was stirred at room temperature for 22 hours. To the reaction mixture, triethylamine (447 μl) was added and the mixture was concentrated. The residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate) to obtain the title compound (1.4 g, 59.1% yield), which is a cis and trans (1:1) mixture, as a light yellow oil.
後処理
- concentrationthe mixture was 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-900281ff6a674c459015a992c92073ad
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07425634B2
反応ノート
読み込み中…