HRID49874

反应详情

EQUATION

反应方程式

HRID 49874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under exclusion of air, 354 mg (2.88 mmol) 4-methoxyaniline and 13 mg lithium iodide are added to 300 mg (0.96 mmol) 7-acetamino-1-chloro-4-(4-pyridylmethyl)phthalazine in 3.9 ml 1-butanol and heated to boiling for 20 h. After cooling, the dark suspension is filtered off, washed with 1-butanol and ethanol, and dried to obtain title compound: m.p.: 160-163° C.; HPLC: tRet(Grad5-40)=9.5; FAB MS (M+H)+=400.

WORKUP

后处理

  1. temperatureheated
  2. temperatureAfter cooling
  3. filtrationthe dark suspension is filtered off
  4. washwashed with 1-butanol and ethanol
  5. customdried