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

HRID 68559

반응식

HRID 68559 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b343e2f0437e49488452de340c3fca77
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822464B2

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