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

HRID 971437ノート

反応式

HRID 971437 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 128147004-(2-fluorophenyl)butan-2-one収率 65.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8562daf21d714fed9030f5276501b741
出典データセット
uspto-grants-1979_07
特許番号
US04160036

反応ノート

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