HRID449643

反应详情

EQUATION

反应方程式

HRID 449643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a 100 mL round bottom flask was added 1-(dimethylamino)-2-methylpropan-2-ol (1.48 g, 12.6 mmol, Eq: 1.5), THF and 3,6-dibromopyridazine (2 g, 8.41 mmol, Eq: 1.00). The flask was cooled to 0° C. followed by addition of NaH (572 mg, 14.3 mmol, Eq: 1.7) in one portion. The turbid reaction mixture was allowed to warm to room temperature and was stirred at room temperature overnight. The resultant black reaction mixture was absorbed onto silica gel and purified by LC chromatography eluting with 0-5% MeOH in 1/1 EtOAc/Hex to afford 1.5 g (65%) of the title compound.

WORKUP

后处理

  1. customThe turbid reaction mixture
  2. temperatureto warm to room temperature
  3. customThe resultant black reaction mixture
  4. customwas absorbed onto silica gel
  5. custompurified by LC chromatography
  6. washeluting with 0-5% MeOH in 1/1 EtOAc/Hex