HRID732133

反应详情

EQUATION

反应方程式

HRID 732133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sulfuryl dichloride (0.58 ml, 8.34 mmol) in DCM (8 ml) was slowly added to a cooled (−10° C.) solution of 4-(4,5-dimethyl-4H-1,2,4-triazol-3-yl)pyridine (454 mg, 2.61 mmol) in DCM (25 ml) and DMF (8 ml) and then the solution was stirred for 2 h. NaHCO3 (sat.) was added and the mixture was extracted with EA. The organic phase was dried and concentrated. Recrystallization from EA afforded 124 mg (23%) of the title compound. 1H NMR: 3.83 (s, 3 H) 4.84 (s, 2 H) 7.62 (d, 2 H) 8.82 (d, 2 H).

WORKUP

后处理

  1. extractionthe mixture was extracted with EA
  2. customThe organic phase was dried
  3. concentrationconcentrated
  4. customRecrystallization from EA