반응 #75596

반응 방정식

3-chloro-3-methyl-1-butyne

4-hydroxypiperidine

→

title compound

1-(1,1-Dimethyl-2-propynyl)-4-piperidinol

용매

diethyl ether

Water

diethyl ether

water

반응 조건

후처리

1. 1
   온도cooled
2. 2
   기타at a bulk temperature of 17 to 22° C
3. 3
   추출the resulting mixture was extracted with diethyl ether for 5 times
4. 4
   건조dried over potassium carbonate
5. 5
   여과over potassium hydroxide, and filtered
6. 6
   농축The filtrate was concentrated at normal pressure
7. 7
   여과The resulting crystalline residues were collected by filtration
8. 8
   workup.ADDITIONby adding ethyl acetate/hexane

실험 절차

24 mg cuprous chloride and 15 mg copper powder were added to a mixed solution of 5 ml solution of 7.3 g 4-hydroxypiperidine in diethyl ether (5 ml) and water (2.5 ml) in a nitrogen atmosphere. The mixture was ice-cooled, and 2.5 ml solution of 2.7 ml 3-chloro-3-methyl-1-butyne in diethyl ether was added dropwise thereinto at a bulk temperature of 17 to 22° C. Then, it was stirred at room temperature overnight. Water was added thereto, and the resulting mixture was extracted with diethyl ether for 5 times. The organic layers were combined, and dried over potassium carbonate and then over potassium hydroxide, and filtered. The filtrate was concentrated at normal pressure. The resulting crystalline residues were collected by filtration by adding ethyl acetate/hexane thereto to give 2.54 g of the title compound.

출처