HRID322217

反应详情

EQUATION

反应方程式

HRID 322217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into an SUS reaction vessel was placed a mixed solvent of 1.5 L of methanol-water (volume ratio 1:2, the same tap water as that used in Example 2 was used as water) into which 99.09 g (1.50 mol) of 50% hydroxylamine aqueous solution was dissolved beforehand. Into the mixed solvent was added 103.56 g (500 mmol) of 2,3-difluoro-6-trifluoromethylbenzonitrile (I″). The reaction temperature stood at 60° C. for 7 hours and was returned to room temperature. In HPLC analysis of the reaction solution, it was shown that (I″) disappeared, 2,3-difluoro-6-trifluoromethylbenzamidoxime (II′) was mainly produced (yield 63.2%) and 2,3-difluoro-6-trifluoromethylbenzamide (III′) was noticeably produced as a byproduct (yield 16.6%).

WORKUP

后处理

  1. customInto an SUS reaction vessel was placed
  2. dissolutionwas dissolved beforehand
  3. customwas returned to room temperature