HRID1383828

反应详情

EQUATION

反应方程式

HRID 1383828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-chloro-4-hydrazinophthalazine hydrochloride (10 g) in dioxan (220 ml) was added triethylamine (7.24 ml) and benzoyl chloride (6.04 ml). This mixture was heated at reflux for 8 hours under nitrogen. After cooling the reaction mixture was concentrated under vacuum and the solid obtained was collected by filtration, washed with water and diethyl ether and dried under vacuum, to yield the title compound (12.0 g). 1H NMR (250 MHz, DMSO) δ 7.60 (3H, m), 8.00 (1H, t, J=8.4Hz), 8.19 (1H, t, J=8.4Hz), 8.31 (3H, m), 8.61 (1H, d, J=6.3Hz).

WORKUP

后处理

  1. temperatureThis mixture was heated
  2. temperatureat reflux for 8 hours under nitrogen
  3. temperatureAfter cooling the reaction mixture
  4. concentrationwas concentrated under vacuum
  5. customthe solid obtained
  6. filtrationwas collected by filtration
  7. washwashed with water and diethyl ether
  8. customdried under vacuum