反応式
[OH:1][CH2:2][C:3]([CH2:8][OH:9])([CH2:6][OH:7])[CH2:4][OH:5].[C:10](OCC)(OCC)(OCC)[CH3:11].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(N(CC)CC)C>>[CH3:10][C:11]12[O:7][CH2:6][C:3]([CH2:8][OH:9])([CH2:4][O:5]1)[CH2:2][O:1]2参加物
5
反応条件
- 温度
- 100 °C
実験手順
A mixture of pentaerythritol (15 g, 110 mmol), triethyl orthoacetate (20.2 ml, 110 mmol), and p-toluenesulfonic acid monohydrate (947 mg, 5.5 mmol) was stirred at 100° C. for 30 minutes. The temperature of the mixture was further raised to 130° C. and the mixture was stirred for 30 minutes. To the reaction mixture, triethylamine (1.53 ml, 11 mmol) was added and the reaction mixture was concentrated. The residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate) to obtain the title compound (8.5 g, yield: 48.2%) as a light yellow solid.
後処理
- temperatureThe temperature of the mixture was further raised to 130° C.
- stirringthe mixture was stirred for 30 minutes
- concentrationthe reaction 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-b4bd0363c7514f7294656ead7bf347c2
- 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…