Acetic Acid → Ethyl 2,4-dichloro-5-fluorobenzoylacetate

HRID 248500

반응식

HRID 248500 반응식
[H-].[Na+].C(O[C:6](=[O:10])[O:7][CH2:8][CH3:9])C.[C:11]([C:14]1[C:19]([Cl:20])=[CH:18][C:17]([Cl:21])=[C:16]([F:22])[CH:15]=1)(=[O:13])[CH3:12].C(O)(=O)C>CCOCC>[Cl:20][C:19]1[CH:18]=[C:17]([Cl:21])[C:16]([F:22])=[CH:15][C:14]=1[C:11]([CH2:12][C:6]([O:7][CH2:8][CH3:9])=[O:10])=[O:13]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 7766Diethyl CarbonateHCID 24758Sodium hydrideHCID 727250Acetophenone, 2',4'-dichloro-5'-fluoro-

생성물 1

HCID 2774350Ethyl 2,4-dichloro-5-fluorobenzoylacetate수율 45%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a suspension of prewashed sodium hydride (76.8 g) in ether was added 189 g of diethylcarbonate. The mixture was heated to reflux and a solution of 131.84 g of 6-acetyl-1,3-dichloro-4-fluorobenzene in 1500 ml of ether was added dropwise over 5 hours. The mixture was then refluxed 24 hours, cooled, poured onto a mixture of ice and acetic acid and extracted several times with ether. The ether extracts were combined, washed with water, dried and evaporated. The residue was purified by vacuum distillation giving 80 g of ethyl 2,4-dichloro-5-fluorobenzoylacetate.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureThe mixture was then refluxed 24 hours
  4. temperaturecooled
  5. extractionextracted several times with ether
  6. washwashed with water
  7. customdried
  8. customevaporated
  9. distillationThe residue was purified by vacuum distillation

출처 및 근거

ORD 기록
ord-27c25f8a47ee49479ecdd224e997d1c6
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210193

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