HRID1809546

反应详情

EQUATION

反应方程式

HRID 1809546 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 2 L flask was charged with 5-bromo-3-phenoxypyridin-2-amine (64.0 g, 241.4 mmol) and benzoyl isothiocyanate (35.82 mL, 265.6 mmol) in THF (600 mL) and stirred at ambient temperature overnight, then concentrated to about 50 mL. A mixture of Hexanes:EtOAc (9:1) (900 mL) was added with vigorous stirring. The resulting suspension was filtered and the solid was washed with hexanes then dried to afford 1-benzoyl-3-(5-bromo-3-phenoxypyridin-2-yl)thiourea (94.32 g, 91.2% yield) as a yellow solid.

WORKUP

后处理

  1. concentrationconcentrated to about 50 mL
  2. additionA mixture of Hexanes:EtOAc (9:1) (900 mL)
  3. additionwas added with vigorous stirring
  4. filtrationThe resulting suspension was filtered
  5. washthe solid was washed with hexanes
  6. customthen dried