반응 #2164

반응 방정식

2-butyne-l,4-diol

3,4-dihydro-2H-pyran

→

4-tetrahydropyranoxy-2-butyn-1-ol

수율 68.8%

용매

ether

ether

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   기타was evaporated
3. 3
   workup.ADDITIONthe residue was poured into 200 ml of water
4. 4
   추출The aqueous solution was extracted with hexane (2×100 ml)
5. 5
   추출re-extracted with ether (3×100 ml)
6. 6
   세척The combined ether extracts were washed with 100 ml of brine
7. 7
   건조dried over magnesium sulfate
8. 8
   기타evaporated

실험 절차

To a mixture of 5.0 g of 2-butyne-l,4-diol and 10 milligrams of p-toluenesulfonic acid and 150 ml of dry ether there was added dropwise with stirring at room temperature 4.9 g of 3,4-dihydro-2H-pyran. After stirring overnight at ambient temperature the ether was evaporated and the residue was poured into 200 ml of water. The aqueous solution was extracted with hexane (2×100 ml) and then re-extracted with ether (3×100 ml). The combined ether extracts were washed with 100 ml of brine, dried over magnesium sulfate and evaporated to yield 6.8 g of 4-tetrahydropyranoxy-2-butyn-1-ol.

출처