반응 #75588

반응 방정식

tert-butyl 4-methylene-1-piperidinecarboxylate

phthalic acid

sodium bicarbonate

→

tert-butyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate

수율 83.6%

용매

methanol

반응 조건

후처리

1. 1
   여과The reaction solution was filtered through Celite
2. 2
   기타the resulting filtrate was evaporated
3. 3
   workup.ADDITIONEthyl acetate was added to the resulting residue which
4. 4
   세척was then washed with water and brine
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   여과filtered
7. 7
   기타The filtrate was evaporated

실험 절차

13.5 g of tert-butyl 4-methylene-1-piperidinecarboxylate was dissolved in 300 ml methanol, and 28.3 g phthalic acid monoperacid magnesium salt and 8.62 g sodium bicarbonate were added thereto, and the mixture was stirred at room temperature for 1 day. The reaction solution was filtered through Celite, and the resulting filtrate was evaporated. Ethyl acetate was added to the resulting residue which was then washed with water and brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated, and subjected to silica gel column chromatography to give 12.2 g of tert-butyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate.

출처