Hydrochloric Acid → 1-Cyclohexyl-3-(4-fluoro-phenyl)-propane-1,3-dione

HRID 68559

反応式

HRID 68559 の反応式
[H-].[Na+].[CH:3]1([C:9](=[O:11])[CH3:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.CO[C:14](=[O:22])[C:15]1[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=1.Cl>C1COCC1>[CH:3]1([C:9](=[O:11])[CH2:10][C:14]([C:15]2[CH:16]=[CH:17][C:18]([F:21])=[CH:19][CH:20]=2)=[O:22])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 13207Cyclohexyl methyl ketoneHCID 24758Sodium hydrideHCID 67878Methyl 4-fluorobenzoate

生成物 1

HCID 867626681-Cyclohexyl-3-(4-fluoro-phenyl)-propane-1,3-dione

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

0.88 g 60% sodiumhydrid was added 1-cyclohexyl-ethanone in 60 mL THF and stirred for 30 min. Then, 3.25 g 4-fluoro-benzoic acid methyl ester and 200 mg 18-Krone-6 was added to the reaction. The reaction was refluxed 2 h and stirred over night at RT. The reaction was added to 100 mL 1N HCl and extracted with diethylether. The organic layer was concentrated and the residue was purified by chromatography on silica gel and 3 g of the desired compound was obtained.

後処理

  1. temperatureThe reaction was refluxed 2 h
  2. stirringstirred over night at RT
  3. extractionextracted with diethylether
  4. concentrationThe organic layer was concentrated
  5. customthe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-b343e2f0437e49488452de340c3fca77
出典データセット
uspto-grants-2014_09
特許番号
US08822464B2

関連ノート

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