反应详情

温度

0 °C

Add 1H-pyrazole-4-carbaldehyde (0.200 g, 2.08 mmol) to a suspension of sodium hydride (0.092 g, 2.29 mmol) in DMF (3 mL) at 0° C. Stir for 20 min. at 0° C. Add a solution of 1-(bromomethyl)cyclopropane (0.295 g, 2.18 mmol) in DMF (4 mL) dropwise to the reaction mixture. Stir reaction to ambient temperature for 18 hr. Quench with aqueous saturated sodium bicarbonate solution and add ethyl acetate. Separate organic layer. Extract aqueous layer twice with ethyl acetate, dry combined organics (magnesium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 0:100 to 60:40 ethyl acetate:hexanes) to give the title preparation (175 mg, 56%). GC-MS: m/z=150 [M+].

1. stirringStir
2. customreaction to ambient temperature for 18 hr
3. customQuench with aqueous saturated sodium bicarbonate solution
4. additionadd ethyl acetate
5. dry with materialExtract aqueous layer twice with ethyl acetate, dry combined organics (magnesium sulfate)
6. filtrationfilter
7. concentrationconcentrate
8. custompurify
9. wash(silica gel chromatography, eluting with 0:100 to 60:40 ethyl acetate:hexanes)
10. customto give the title
11. custompreparation (175 mg, 56%)