反应详情

温度

0 °C

Add 1H-pyrazole-4-carbaldehyde (0.400 g, 4.16 mmol) as a solution in DMF (2 mL) dropwise to a suspension of sodium hydride (0.333 g, 8.32 mmol) in DMF (5 mL) at 0° C. Stir for 15 min. at 0° C. Add 2,2,2-trifluoroethyl-p-toluenesulfonate (1.27 g, 5.00 mmol) and DMF (3 mL) to the reaction mixture. Heat to 60° C. for 18 hr. Quench with aqueous saturated sodium bicarbonate solution and add ethyl acetate. Separate organic layer. Extract aqueous layer twice with ethyl acetate, wash combined organics with brine, dry (magnesium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 0:100 to 100:0 ethyl acetate:hexanes) to give the title preparation (309 mg, 42%). GC-MS: m/z=178 [M+].

1. temperatureHeat to 60° C. for 18 hr
2. customQuench with aqueous saturated sodium bicarbonate solution
3. additionadd ethyl acetate
4. washExtract aqueous layer twice with ethyl acetate, wash
5. dry with materialdry (magnesium sulfate)
6. filtrationfilter
7. concentrationconcentrate
8. custompurify
9. wash(silica gel chromatography, eluting with 0:100 to 100:0 ethyl acetate:hexanes)
10. customto give the title
11. custompreparation (309 mg, 42%)