반응 #2265

반응 방정식

cyclohexylacetylene

formaldehyde

paraformaldehyde

→

3-cyclohexyl-2-propyn-1-ol

용매

ether

ether

반응 조건

후처리

1. 1
   온도the reaction mixture was refluxed for 2 hours
2. 2
   기타was bubbled into the mixture
3. 3
   온도After cooling
4. 4
   기타the reaction was quenched with saturated ammonium chloride
5. 5
   추출extracted with ether (2×100 ml)
6. 6
   세척The combined ether extracts were washed with brine
7. 7
   건조dried over magnesium sulfate
8. 8
   기타evaporated
9. 9
   기타to yield the product which
10. 10
    workup.DISTILLATIONwas distilled under high vacuum at 68°-74° C.
11. 11
    기타to yield 6.4 g as a colorless liquid

실험 절차

To a solution of ethyl magesium bromide (prepared from 2.5 g of magnesium turning and 11.3 g of bromoethane) in ether was added dropwise a solution of 10.2 g of cyclohexylacetylene in ether and the reaction mixture was refluxed for 2 hours. The reaction mixture was cooled to ambient temperature and anhydrous formaldehyde (prepared from the thermal decomposition of 50 g of paraformaldehyde for 20 minutes) was bubbled into the mixture. After cooling, the reaction was quenched with saturated ammonium chloride and extracted with ether (2×100 ml). The combined ether extracts were washed with brine, dried over magnesium sulfate and evaporated to yield the product which was distilled under high vacuum at 68°-74° C. to yield 6.4 g as a colorless liquid.

출처