HRID712148

反应详情

EQUATION

反应方程式

HRID 712148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of 3-benzyloxy-5-bromo-aniline (480 g, 1.73 mol) in acetone (10 L) was added benzoylisothiocyanate (280 mL, 2.08 mol) at rt. After stirring the reaction mixture for 15 min, solid precipitated out and stirring was continued for 30 min at rt. After completion of reaction (by TLC), acetone was distilled off. Hexane (2 L) was added and again concentrated. To the concentrated solid was added hexane (4 L) heated to 40° C. for 30 min under stirring and the solid filtered. The solid was washed with hexane (2×2 L) to obtain the desired product (648 g, 85%).

WORKUP

后处理

  1. customsolid precipitated out
  2. stirringstirring
  3. waitwas continued for 30 min at rt
  4. customAfter completion of reaction (by TLC), acetone
  5. distillationwas distilled off
  6. additionHexane (2 L) was added
  7. concentrationagain concentrated
  8. additionTo the concentrated solid was added hexane (4 L)
  9. stirringunder stirring
  10. filtrationthe solid filtered
  11. washThe solid was washed with hexane (2×2 L)