2-Butyne-1,4-diol → 4-(Tetrahydro-pyran-2-yloxy)-but-2-yn-1-ol

To a mixture of 5.0 g of 2-butyne-1,4-diol and 10 milligrams of p-toluenesulfonic add 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.

1. additionof p-toluenesulfonic add
2. customwas evaporated
3. additionthe residue was poured into 200 ml of water
4. extractionThe aqueous solution was extracted with hexane (2×100 ml)
5. extractionre-extracted with ether (3×100 ml)
6. washThe combined ether extracts were washed with 100 ml of brine
7. dry with materialdried over magnesium sulfate
8. customevaporated

ORDレコード

ord-65c75dc89f17409bb6ee8bc64675c761

出典データセット

uspto-grants-1998_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05726162