반응 #75910

반응 방정식

p-Fluorobenzaldehyde

propionic anhydride

sodium propionate

→

p-Fluoro-α-methylcinnamic acid

반응 조건

후처리

1. 1
   기타had been flushed with nitrogen
2. 2
   온도the flask is cooled to 100° C.
3. 3
   workup.ADDITIONpoured into 8 l of water
4. 4
   workup.DISSOLUTIONThe precipitate is dissolved
5. 5
   workup.ADDITIONby adding potassium hydroxide (302 g) in 2 l of water
6. 6
   추출The aqueous solution is extracted with ether
7. 7
   세척the ether extracts are washed with potassium hydroxide solution
8. 8
   여과The combined aqueous layers are filtered
9. 9
   여과are filtered
10. 10
    세척The collected solid, p-fluoro-α-methylcinnamic acid, is washed with water
11. 11
    기타is dried
12. 12
    기타as obtained

실험 절차

p-Fluorobenzaldehyde (200 g, 1.61 mol), propionic anhydride (3.5 g, 2.42 mol) and sodium propionate (155 g, 1.61 mol) are mixed in a one liter three-necked flask which had been flushed with nitrogen. The flask is heated gradually in an oil-bath to 140° C. After 20 hours, the flask is cooled to 100° C. and poured into 8 l of water. The precipitate is dissolved by adding potassium hydroxide (302 g) in 2 l of water. The aqueous solution is extracted with ether, and the ether extracts are washed with potassium hydroxide solution. The combined aqueous layers are filtered, are acidified with concentrated HCl, and are filtered. The collected solid, p-fluoro-α-methylcinnamic acid, is washed with water, and is dried and used as obtained.

출처