HRID66649

反应详情

EQUATION

反应方程式

HRID 66649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

4-Fluoropiperidine (0.7 g., 0.005 mole) was dissolved in a mixture of 3 ml. of dioxane and 2 ml. of water containing cyanoacetic acid (0.43 g., 0.005 mole). The solution was heated to 65° C. and carbon dioxide evolution began. It was maintained at 60°-65° C. for 21/2 hours and allowed to stand overnight. A solid gummy residue, 1 gm., was obtained upon stripping in a bath at 55° C. and at 1 mm. It was taken up in a small amount of water, made alkaline with sodium bicarbonate and extracted with ether. The organic layer was water washed and dried over anhydrous sodium sulfate. After solvent stripping, the product was obtained as a colorless oil, 0.7 g., of analytical purity.

WORKUP

后处理

  1. temperatureIt was maintained at 60°-65° C. for 21/2 hours
  2. custom, was obtained
  3. customupon stripping in a bath at 55° C. and at 1 mm
  4. extractionextracted with ether
  5. washwashed
  6. dry with materialdried over anhydrous sodium sulfate
  7. customAfter solvent stripping, the product was obtained as a colorless oil, 0.7 g