反応 #7427

反応方程式

2,3-dihydropyran

p-hydroxybenzoic acid

methylene chloride

→

p-tetrahydropyranyloxy benzoic acid

収率 86.2%

溶媒

ether

反応条件

後処理

1. 1
   workup.DISSOLUTIONThe mixture was dissolved
2. 2
   抽出it was extracted 3 times with 70 ml of a 10% sodium hydroxide aqueous solution
3. 3
   抽出The resulting extracted solution
4. 4
   ろ過The resulting precipitate was filtered
5. 5
   その他dried in a vacuum

実験手順

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.

出典