1,2-Dichloroethane → Methyl 6-methylpyridine-2-carboxylate
反応式
[CH3:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][CH:3]=1.CO.[CH2:13](Cl)CCl>C(Cl)Cl.CN(C)C1C=CN=CC=1>[CH3:13][O:9][C:8]([C:6]1[CH:5]=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=1)=[O:10]参加物
6
反応条件
- 温度
- 0 °C
実験手順
To a suspension of 6-methyl-pyridine-2-carboxylic acid (10 g, 72.9 mmol) in methylene chloride (200 mL) cooled to 0° C. is added methanol (10 mL), 4-dimethylaminopyridine (11.6 g, 94.8 mmol), and EDC (18.2 g, 94.8 mmol). The mixture is stirred at room temperature for 6 h, washed with water and brine, and dried over sodium sulfate. The mixture is filtered and concentrated in vacuo. The residue is chromatographed on SiO2 (50% ethyl acetate/hexanes) to yield the title compound, 9.66 g (92%), as a colorless liquid.
後処理
- washwashed with water and brine
- dry with materialdried over sodium sulfate
- filtrationThe mixture is filtered
- concentrationconcentrated in vacuo
- customThe residue is chromatographed on SiO2 (50% ethyl acetate/hexanes)
出典と根拠
- ORDレコード
- ord-6f91fd8aa044449a8fb53ad9db2adc17
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07087626B2
反応ノート
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