HRID913873

反应详情

EQUATION

反应方程式

HRID 913873 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 5-chloro-1H-indazole-7-carbaldehyde (1.0 g, 5.54 mmol) in acetic acid (5 mL) was added bromine (0.43 mL, 8.31 mmol) slowly over 5 min. After 1 h, the reaction mixture was diluted with methylene chloride, washed with water (2×), saturated sodium thiosulfate (2×), saturated sodium bicarbonate (2×), then brine (2×), dried over sodium sulfate, and concentrated to afford 1.4 g (97%) as a yellow powder. LC/MS (HPLC method 1): tR=2.49 min, 261.00(MH)+.

WORKUP

后处理

  1. washwashed with water (2×), saturated sodium thiosulfate (2×), saturated sodium bicarbonate (2×)
  2. dry with materialbrine (2×), dried over sodium sulfate
  3. concentrationconcentrated
  4. customto afford 1.4 g (97%) as a yellow powder