HRID2239888

反应详情

EQUATION

反应方程式

HRID 2239888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a 25 mL flask was added 3-(3-chlorophenyl)furan-2,5-dione (1.7 g, 8.15 mmol) from (1a) and hydrazine hydrate (0.476 mL, 9.78 mmol) in water (6 mL) and acetic acid (4 mL). The resulting mixture was refluxed for 18 hours. The solution was cooled and placed in the refrigerator for 1 hour. The resulting precipitate was filtered and dried, then purified by flash chromatography eluting with 5% methanol/dichloromethane to give 4-(3-chlorophenyl)pyridazine-3,6-diol.

WORKUP

后处理

  1. temperatureThe resulting mixture was refluxed for 18 hours
  2. temperatureThe solution was cooled
  3. filtrationThe resulting precipitate was filtered
  4. customdried
  5. custompurified by flash chromatography
  6. washeluting with 5% methanol/dichloromethane