HRID1606596

反应详情

EQUATION

反应方程式

HRID 1606596 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

(3-Trifluoromethylphenoxy)(4-chlorophenyl)acetonitrile is added to a solution of 2-acetamidoethanol (20.6 g., 0.2 mole) in anhydrous dimethylformamide (25 ml.). The reaction mixture is cooled to -10°C. and saturated with hydrogen chloride (50 g., 1.37 mole) and stirred for 5 hours at -10° to 0°C. To this reaction mixture containing 2-acetamidoethyl (3-trifluoromethylphenoxy)(4-chlorophenyl)iminoacetate hydrochloride is added methylene chloride (200 ml.) and then water (100 ml.). The organic layer is collected, washed with water (2 × 100 ml.) and then dried over magnesium sulfate. The dried solution is decolorized with carbon, filtered and then slowly diluted with hexane (1 liter) to afford 10.7 g. (25% yield) of 2-acetamidoethyl (3-trifluoromethylphenoxy)(4-chlorophenyl)acetate, m.p. 93°-95°C.

WORKUP

后处理

  1. customThe organic layer is collected
  2. washwashed with water (2 × 100 ml.)
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. additionslowly diluted with hexane (1 liter)
  6. customto afford 10.7 g