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(4-fluoro-phenyl)-hydrazine hydrochloride[ No CAS ]
[ 120-92-3 ]
[ 327021-84-1 ]
Yield
Reaction Conditions
Operation in experiment
62%
With sulfuric acid; In isopropyl alcohol; at 100℃; for 1.0h;
4-fluorophenylhydrazine hydrochloride 1.00 g (6.2 mmol),Cyclopentanone 0.52g (6.2mmol),31 mL of isopropanol was added to the reaction tube with a branch pipe,Degas completely,0.7 mL of degassed concentrated sulfuric acid was added dropwise at room temperature.After the completion of the dropwise addition, the temperature was raised to 100 C for 1 h.After the reaction is completed, the reaction solution is poured into 100 mL of water.Extracted with dichloromethane (3 x 30 mL),The organic phase is combined and dried,filter,The solvent was removed under reduced pressure.Column chromatography (PE: DCM = 1:1),Obtained white solid 0.67g,The yield was 62%.
With palladium on activated charcoal; hydrogen; In tetrahydrofuran; for 24.0h;
37 0.75g (4.3mmol) was added to the two-necked flask,Add 25 mL of tetrahydrofuran,After the dissolution was completed, 0.20 g of Pd/C catalyst was added.The reaction was stirred with hydrogen for 24 h.After the reaction is completed, the filter is filtered to remove Pd/C.The filtrate is distilled off under reduced pressure,Column chromatography (PE to PE: DCM=1:1),Obtained 0.46g of colorless oily liquid,The yield was 61%.
Chemistry
Pharmaceutical Intermediates
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Material Science
For Research Only
110K+ Compounds
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