反应详情

A mixture of 1H-pyrazole (6.00 g, 88.1 mmol), 3,4-dihydro-2H-pyran (9.00 g, 107 mmol), and TFA (cat. 2.00 mL) was heated to reflux for 5 hr. At the end of reaction, NaH (100 mg, 4.17 mmol) was added to quench the reaction. The resulting mixture was extracted with ethyl acetate, washed with brine, dried over MgSO4, filtered, and evaporated. The residue was purified by silica gel chromatography eluting with EtOAc/petroleum ether (1:100) to afford 1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole (6.6 g, 49% yield) as pale yellow sold. LCMS (ESI) m/z: 153.1 [M+H+].

1. temperaturewas heated
2. temperatureto reflux for 5 hr
3. additionwas added
4. customto quench
5. customthe reaction
6. extractionThe resulting mixture was extracted with ethyl acetate
7. washwashed with brine
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. customevaporated
11. customThe residue was purified by silica gel chromatography
12. washeluting with EtOAc/petroleum ether (1:100)