HRID2064645

反应详情

EQUATION

反应方程式

HRID 2064645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-methoxy-1H-indazole [0.815 g, Reference Example 24(a)] in dimethyl formamide (8 ml) was treated with iodine (2.80 g) and potassium hydroxide (1.16 g). The mixture was stirred at ambient temperature for 1 hour then poured into 10% aqueous sodium bisulfite solution (200 ml) and then extracted three times with ethyl acetate. The combined organic extracts were washed with water, then with brine, then dried over magnesium sulfate and then evaporated to yield 3-iodo-5-methoxy-1H-indazole (1.48 g) as a yellow solid. LC-MS (METHOD B): RT=2.96 minutes; 275 (M+H)+.

WORKUP

后处理

  1. extractionextracted three times with ethyl acetate
  2. washThe combined organic extracts were washed with water
  3. dry with materialwith brine, then dried over magnesium sulfate
  4. customevaporated