Propionic anhydride → CID 367964

HRID 47632

반응식

HRID 47632 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[CH:4][CH:3]=1.[C:10]([O:14]C(=O)CC)(=[O:13])[CH2:11][CH3:12].C([O-])(=O)CC.[Na+]>>[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[C:11]([CH3:12])[C:10]([OH:14])=[O:13])=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 31263Propionic anhydrideHCID 680234-FluorobenzaldehydeHCID 2723816Sodium Propionate

생성물 1

HCID 367964CID 367964

반응 조건

온도
140 °C

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.

후처리

  1. customhad been flushed with nitrogen
  2. temperaturethe flask is cooled to 100° C.
  3. additionpoured into 8 l of water
  4. dissolutionThe precipitate is dissolved
  5. additionby adding potassium hydroxide (302 g) in 2 l of water
  6. extractionThe aqueous solution is extracted with ether
  7. washthe ether extracts are washed with potassium hydroxide solution
  8. filtrationThe combined aqueous layers are filtered
  9. filtrationare filtered
  10. washThe collected solid, p-fluoro-α-methylcinnamic acid, is washed with water
  11. customis dried
  12. customas obtained

출처 및 근거

ORD 기록
ord-6efc3b3c28c54bd1a91d9c35dff01a04
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699894B1

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