반응 #7427

반응 방정식

2,3-dihydropyran

p-hydroxybenzoic acid

methylene chloride

→

p-tetrahydropyranyloxy benzoic acid

수율 86.2%

용매

ether

반응 조건

후처리

1. 1
   workup.DISSOLUTIONThe mixture was dissolved
2. 2
   추출it was extracted 3 times with 70 ml of a 10% sodium hydroxide aqueous solution
3. 3
   추출The resulting extracted solution
4. 4
   여과The resulting precipitate was filtered
5. 5
   기타dried in a vacuum

실험 절차

Into a 300 ml three neck flask were charged 25.4 g of 2,3-dihydropyran (reagent, manufactured by Tokyo Kasei Kogyo Co., Ltd.), 41.4 g of p-hydroxybenzoic acid (reagent, manufactured by Tokyo Kasei Kogyo Co., Ltd.), and 3.7 g of pyridinium p-toluenesulfonate (reagent, manufactured by Tokyo Kasei Kogyo Co., Ltd.). The mixture was dissolved after addition of 20 ml of methylene chloride and 80 ml of absolute ether. After the mixture was vigorously stirred for about 3 hours, it was extracted 3 times with 70 ml of a 10% sodium hydroxide aqueous solution. The resulting extracted solution was neutralized with 1 N of hydrochloric acid until the pH is made to 6. The resulting precipitate was filtered and dried in a vacuum thereby obtaining 57.4 g of crude p-tetrahydropyranyloxy benzoic acid.

출처