HRID1919687

反应详情

EQUATION

反应方程式

HRID 1919687 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Methyl 5-(3-chlorophenylamino)benzo[c][2,6]naphthyridine-7-carboxylate (47 mg) was mixed with Methanol (1 ml) and Hydrazine hydrate (1 ml). 2-3 drops of DMF were added and the mixture was stirred at 60° C. for 2 hours. The volatiles were removed and another amount of reagent Methanol (1 ml) and Hydrazine (1 ml) were added, and the mixture was stirred at 60° C. for an extra 2 hours. The volatiles were removed in vacuo and the material was crashed out using AcOEt/hexanes. Filtration and drying afforded 5-(3-chlorophenylamino)benzo[c][2,6]naphthyridine-7-carbohydrazide as a solid (29 mg, 62% yield). LCMS (ES): >85% pure, m/z 364 [M+1]+.

WORKUP

后处理

  1. customThe volatiles were removed
  2. additionanother amount of reagent Methanol (1 ml) and Hydrazine (1 ml) were added
  3. stirringthe mixture was stirred at 60° C. for an extra 2 hours
  4. customThe volatiles were removed in vacuo
  5. filtrationFiltration
  6. customdrying