Benzene, 1-(chloromethyl)-2-fluoro- → 4-(2-fluorophenyl)butan-2-one

HRID 971437노트

반응식

HRID 971437 반응식
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4]Cl.[C:10]([CH2:13]C(=O)C)(=[O:12])[CH3:11].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][CH2:11][C:10](=[O:12])[CH3:13]

참가 물질

5

반응물 3

HCID 9580Benzene, 1-(chloromethyl)-2-fluoro-HCID 11430Potassium CarbonateHCID 31261Acetylacetone

생성물 1

HCID 128147004-(2-fluorophenyl)butan-2-one수율 65.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A stirred mixture of 2-fluorobenzyl chloride (22.47 g), acetylacetone (17.10 g), anhydrous potassium carbonate (21.5 g) and ethanol (155 ml) was heated at reflux for 18 hr. The solvent was evaporated and the residue was partitioned between water (200 ml) and ether (150 ml). The aqueous layer was washed with ether (3×150 ml). The extracts were combined, washed with brine (200 ml), dried (MgSO4) and evaporated. Distillation of the residue under reduced pressure gave the product (17 g) b.p. 58°-66°/0.5-0.6 mm.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 18 hr
  3. customThe solvent was evaporated
  4. customthe residue was partitioned between water (200 ml) and ether (150 ml)
  5. washThe aqueous layer was washed with ether (3×150 ml)
  6. washwashed with brine (200 ml)
  7. dry with materialdried (MgSO4)
  8. customevaporated
  9. distillationDistillation of the residue under reduced pressure

출처 및 근거

ORD 기록
ord-8562daf21d714fed9030f5276501b741
출처 데이터셋
uspto-grants-1979_07
특허 번호
US04160036

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