HRID6719

反应详情

EQUATION

反应方程式

HRID 6719 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of trans-N-[4-(3-chlorophenyl)-but-3-enyl]-phthalimide (0.50 g) and methylamine (2 M in tetrahydrofuran, 8 mL) in 20 mL ethanol was heated to reflux for 4 h. The solution was cooled to rt and the solvent was removed in vacuo. The resulting residue was dissolved in ethyl acetate and extracted 3 times with 1 M hydrochloric acid. The combined acid layers were made basic with potassium hydroxide to pH 9 and extracted with ethyl acetate. The ethyl acetate layer was dried over sodium sulfate and the solvent was removed in vacuo to yield 0.20 g of trans-4-(3-chlorophenyl)-but-3-enylamine.

WORKUP

后处理

  1. temperatureto reflux for 4 h
  2. customthe solvent was removed in vacuo
  3. dissolutionThe resulting residue was dissolved in ethyl acetate
  4. extractionextracted 3 times with 1 M hydrochloric acid
  5. extractionextracted with ethyl acetate
  6. dry with materialThe ethyl acetate layer was dried over sodium sulfate
  7. customthe solvent was removed in vacuo