HRID876524

反应详情

EQUATION

反应方程式

HRID 876524 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

2-acetyl-6-nitrophenyl nicotinate 5 (1.3 g, 4.4 mmol) was dissolved in pyridine (10 mL) and heated to 50° C. Finely powdered KOH (3.4 g, 6.1 mmol) was added in small portions. After cooling to room temperature the reaction mixture was concentrated to dryness. Concentrated H2SO4 (0.4 g, 4.4 mmol) and AcOH (3 mL) was added and the mixture was heated to 80° C. for 2 h. The reaction mixture was concentrated to dryness and the crude residue was purified by flash chromatography eluting with Pentane/EtOAc (5:1) to give 6 (410 mg, 35% yield).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature the reaction mixture
  2. concentrationwas concentrated to dryness
  3. temperaturethe mixture was heated to 80° C. for 2 h
  4. concentrationThe reaction mixture was concentrated to dryness
  5. customthe crude residue was purified by flash chromatography
  6. washeluting with Pentane/EtOAc (5:1)