HRID1808554

反应详情

EQUATION

反应方程式

HRID 1808554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

4-(Methyloxy)-1H-indazol-3-amine (for a preparation see Intermediate 1) (500 mg, 3 mmol) and phthalic anhydride (680 mg, 4.6 mmol) (available from Aldrich) were dissolved in 1,4-dioxane (5 mL) at room temperature. The reaction mixture was stirred at 110° C. overnight, and then it was cooled and concentrated under reduced pressure. The residue was triturated and sonicated with 50 mL of ether. The solid was collected by filtration and dried in a vacuum oven to obtain a brown solid (711 mg, 81%). LCMS (System B) RT=2.82 min, ES+ve m/z 294 (M+H)+.

WORKUP

后处理

  1. temperatureit was cooled
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was triturated
  4. customsonicated with 50 mL of ether
  5. filtrationThe solid was collected by filtration
  6. customdried in a vacuum oven