반응 #640617

반응 방정식

potassium tert-butylate

1-boc-4-piperidone

NH4Cl

→

4-methylene-piperdine-1-carboxylic acid tert-butylester

용매

diethylether

diethylether

반응 조건

후처리

1. 1
   workup.ADDITIONwas slowly added
2. 2
   workup.STIRRINGThe suspension was stirred for a further 30 min at 0° C
3. 3
   기타the organic phase was separated
4. 4
   건조dried over magnesium sulphate
5. 5
   기타the solvent removed under vacuum

실험 절차

1.6 g (14 mmol) potassium tert-butylate were added while stirring at 0° C. (ice bath) to a suspension of 5.34 g (15 mmol) methyltriphenylphosphonium bromide in 50 ml diethylether. After stirring for 15 minutes a solution of 2.00 g (10 mmol) 1-boc-4-piperidone (from Merck KGaA) in 15 mmol diethylether was slowly added. The suspension was stirred for a further 30 min at 0° C. After adding 60 ml 10% aqueous NH4Cl solution, the organic phase was separated, dried over magnesium sulphate and the solvent removed under vacuum. After chromatography on silica gel (hexane:ethylacetate=5:1) 1.71 g (89%) 4-methylene-piperdine-1-carboxylic acid tert-butylester were obtained as a colorless liquid.

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