反応 #6655
ord-8a817766383541e695f1bd93a0b40edf
反応方程式
6-chloronicotinic acid
ethanol
dicyclohexylcarbodiimide
dimethylaminopyridine
→
title compound
Ethyl 6-chloronicotinate
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度was heated
- 2温度at reflux for 2 hours
- 3温度to cool
- 4その他solvent removed in vacuo
実験手順
A mixture of 15.75 g (0.1 mol) 6-chloronicotinic acid, 6.9 g (0.15 mol) ethanol, 22.7 g (0.11 mol) dicyclohexylcarbodiimide and 3.7 g dimethylaminopyridine in 200 ml methylene chloride was heated at reflux for 2 hours. The mixture was allowed to cool, solvent removed in vacuo and the residue subjected to flash chromatography to give the title compound as a low-melting white solid. PMR (CDCl3): δ 1.44 (3H, t, J~6.2 Hz) 4.44 (2H, q, J~4.4 Hz), 7.44 (1H, d, J~8.1 Hz), 8.27 (1H, dd, J~8.1 Hz, 3 Hz), 9.02 (1H, d, J~3 Hz).