反応 #8305

ord-6f91fd8aa044449a8fb53ad9db2adc17

反応方程式

Cc1cccc(C(=O)O)n1
6-methyl-pyridine-2-carboxylic acid
CO
methanol
ClCCCl
EDC
COC(=O)c1cccc(C)n1
title compound
COC(=O)c1cccc(C)n1
6-Methyl-pyridine-2-carboxylic acid methyl ester

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with water and brine
  2. 2
    乾燥dried over sodium sulfate
  3. 3
    ろ過The mixture is filtered
  4. 4
    濃縮concentrated in vacuo
  5. 5
    その他The residue is chromatographed on SiO2 (50% ethyl acetate/hexanes)

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087626B2uspto-grants-2006_08