HRID876523

反应详情

EQUATION

反应方程式

HRID 876523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1-(2-Hydroxy-3-nitrophenyl)ethanone 1 (1.0 g, 5.5 mmol), nicotinic acid 4 (0.8 g, 5.8 mmol), DCC (2.4 g, 11.6 mmol) and DMAP (0.7 g, 5.8 mmol) in CH2Cl2 (30 mL) was stirred at room temperature for 12 hours. After cooling to 0° C., the precipitated dicyclohexyl urea was removed by filtration and the filtrate concentrated. The crude residue was purified by flash chromatography eluting with Pentane/EtOAc (10:1) to give 5 (1.3 g, 81% yield).

WORKUP

后处理

  1. temperatureAfter cooling to 0° C.
  2. customthe precipitated dicyclohexyl urea was removed by filtration
  3. concentrationthe filtrate concentrated
  4. customThe crude residue was purified by flash chromatography
  5. washeluting with Pentane/EtOAc (10:1)