HRID1680857

反应详情

EQUATION

反应方程式

HRID 1680857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.8 g of magnesium are covered with 10 ml of absolute tetrahydrofuran. About 1 ml of a solution of 8 g of vinyl bromide in 8 ml of absolute tetrahydrofuran is added dropwise and the reaction is initiated by slight warming. Then, the remainder of the vinyl bromide solution is added dropwise. The mixture is left to react until it reaches room temperature. A solution of 7 g of 2-naphthaldehyde in 50 ml of absolute tetrahydrofuran is then added slowly dropwise, as the temperature rises to 40° C. The reaction is completed within 1 hour. The mixture is then hydrolyzed by the addition with stirring of 20 ml of saturated ammonium chloride solution at 0° C. The residue is filtered and rinsed with ether. The filtrate is diluted with water and extracted twice with ether. The ether extracts are washed with semi-saturated and saturated sodium chloride solution, dried over sodium sulfate and evaporated to yield 1-(2-naphthyl)-2-propen-1-ol which, without further purification, is esterified with cyclopropane carboxylic acid chloride in the process of Example 2. The resulting product is cyclopropane carboxylic acid 1-(2-naphthyl)allyl ester of melting point 30°-32° C.

WORKUP

后处理

  1. waitThe mixture is left
  2. customto react until it
  3. customreaches room temperature
  4. customrises to 40° C
  5. additionThe mixture is then hydrolyzed by the addition
  6. filtrationThe residue is filtered
  7. washrinsed with ether
  8. additionThe filtrate is diluted with water
  9. extractionextracted twice with ether
  10. washThe ether extracts are washed with semi-saturated and saturated sodium chloride solution
  11. dry with materialdried over sodium sulfate
  12. customevaporated