反应 #2225

反应方程式

3-(3-chlorobenzoyl)propionic acid

potassium hydroxide

hydrazine

→

product

收率 90.8%

4-(3-chlorophenyl)-butyric acid

收率 90.8%

溶剂

diethyleneglycol

反应条件

后处理

1. 1
   其他To a 300 ml round-bottomed flask equipped with magnetic stirrer
2. 2
   温度reflux condenser
3. 3
   温度The mixture was heated
4. 4
   其他was azeotroped off into a Dean-Stark trap
5. 5
   温度The reaction was refluxed for an additional 2 hours
6. 6
   温度cooled
7. 7
   workup.ADDITIONpoured into 500 g of ice with 50 ml of con
8. 8
   其他A white precipitate was formed which
9. 9
   萃取was extracted into 400 ml of ethyl ether
10. 10
    洗涤washed with 100 ml of water and 100 ml of saturated sodium chloride solution
11. 11
    萃取The ether extract
12. 12
    干燥was dried over anhydrous magnesium sulfate
13. 13
    过滤filtered

实验过程

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.

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