반응 #1611

반응 방정식

3-(3-chlorobenzoyl)-propionic acid

potassium hydroxide

hydrazine

→

product

수율 90.8%

4-(3-chlorophenyl)-butyric acid

수율 90.8%

용매

diethyleneglycol

반응 조건

후처리

1. 1
   기타To a 300 ml round-bottomed flask equipped with magnetic stirrer
2. 2
   온도reflux condenser
3. 3
   온도The mixture was heated
4. 4
   기타was azeotroped off into a Dean-Stark trap
5. 5
   온도The reaction was refluxed for an additional 2 hours
6. 6
   온도cooled
7. 7
   workup.ADDITIONpoured into 500 g of ice with 50 ml of con
8. 8
   기타A white precipitate was formed which
9. 9
   추출was extracted into 400 ml of ethyl ether
10. 10
    세척washed with 100 ml of water and 100 ml of saturated sodium chloride solution
11. 11
    추출The ether extract
12. 12
    건조was dried over anhydrous magnesium sulfate
13. 13
    여과filtered

실험 절차

To a 300 ml round-bottomed flask equipped with magnetic stirrer and reflux condenser was charged 23.7 g of 87% potassium hydroxide and 150 ml of diethyleneglycol, With stirring, 23 g of 3-(3-chlorobenzoyl)-propionic acid was added followed by 24 g of 85% hydrazine. The mixture was heated to reflux for 2 hours when 50 ml of solvent was azeotroped off into a Dean-Stark trap. The reaction was refluxed for an additional 2 hours, cooled, and poured into 500 g of ice with 50 ml of con. hydrochloric acid. A white precipitate was formed which was extracted into 400 ml of ethyl ether, and washed with 100 ml of water and 100 ml of saturated sodium chloride solution. The ether extract was dried over anhydrous magnesium sulfate, filtered, and stripped to yield 19.5 g of product as a white solid.

출처