HRID1514391

反应详情

EQUATION

反应方程式

HRID 1514391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a round bottomed flask containing 3-benzoylpicolinic acid (2.00 g, 9 mmol) was added 50 mL of ethanol. Hydrazine hydrate (0.6 ml, 11 mmol) was added and the mixture was heated to reflux for 3 h. After cooling to rt, the solvent was removed in vacuo. The resulting yellow solid was recrystallized from 30 mL of boiling 1-propanol to afford 5-phenylpyrido[2,3-d]pyridazin-8(7H)-one 70 (1.4 g, 71% yield) as a white solid. 1H-NMR (400 MHz, CDCl3): δ 10.55 (br s, 1H), 9.16 (dd, J=8.6, 1.6 Hz, 1H), 7.73 (dd, J=8.6, 4.7 Hz, 1H), 7.56 (m, 5H).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 3 h
  3. customthe solvent was removed in vacuo
  4. customThe resulting yellow solid was recrystallized from 30 mL of boiling 1-propanol