Propionic anhydride → CID 367964

HRID 377739

반응식

HRID 377739 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 nitrogen-flushed 1 l three-necked flask. The flask is heated gradually in an oil-bath to 140° C. After 20 hours, the contents are cooled to 100° C., and are poured into 8 l of water. The precipitate is dissolved by adding potassium hydroxide (302 g) in water (2 l). The aqueous solution is washed with ether, and the ether layers are re-extracted 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. customflushed 1 l three-necked flask
  2. temperaturethe contents are cooled to 100° C.
  3. additionare poured into 8 l of water
  4. dissolutionThe precipitate is dissolved
  5. additionby adding potassium hydroxide (302 g) in water (2 l)
  6. washThe aqueous solution is washed with ether
  7. extractionthe ether layers are re-extracted 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-e642dff59c424e39ab57fa83802bb7cb
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06028116

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