HRID245791

反应详情

EQUATION

反应方程式

HRID 245791 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a round-bottomed flask, 6-chloro-1H-indazole (90 mg, 0.59 mmol) was dissolved in DMF (1.4 mL). Iodine (300 mg, 1.18 mmol) was added followed by potassium hydroxide (128 mg, 2.28 mmol). The dark reaction mixture was stirred at room temperature for 3 h then was quenched with 10% aq NaHSO3 and extracted with diethyl ether (2×). The combined organic layers were washed with water and brine then dried over sodium sulfate, filtered and concentrated to give 169 mg (98%) of 6-chloro-3-iodo-1H-indazole as an orange solid.

WORKUP

后处理

  1. customThe dark reaction mixture
  2. customthen was quenched with 10% aq NaHSO3
  3. extractionextracted with diethyl ether (2×)
  4. washThe combined organic layers were washed with water and brine
  5. dry with materialthen dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated