反应详情

温度

60 °C

To a solution of Example B1 (10.00 g, 46.4 mmol, 1.00 eq) and pyridine (7.58 ml, 92.9 mmol, 2.00 eq) in CH2Cl2 (225 ml) at 0° C. was added isopropenyl chloroformate (5.33 ml, 4.8.8 mol, 1.05 eq). After 45 min at 0° C., the completed reaction was washed with 3M HCl (2×), satd. NaHCO3 (1×), and brine (1×), dried (MgSO4), filtered and evaporated to afford crude product (14.9 g) as an oil that solidified on the pump. The crude material obtained was upgraded by triturating in warm (60° C.) hexanes (70 ml) for 20-30 min until a powdery precipitate was obtained. After cooling to RT, the solids were collected by filtration, rinsing forward with hexanes. The cake was washed with more hexanes and then dried on the filter to afford prop-1-en-2-yl 3-t-butyl-1-phenyl-1H-pyrazol-5-ylcarbamate (10.79 g, 78% yield) as a tan powder which was used as is in the next reaction. MS (ESI) m/z: 300.3 (M+H+).

1. customthe completed reaction
2. washwas washed with 3M HCl (2×)
3. dry with materialNaHCO3 (1×), and brine (1×), dried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customto afford crude product (14.9 g) as an oil that
7. customThe crude material obtained
8. customby triturating
9. customwas obtained
10. temperatureAfter cooling to RT
11. filtrationthe solids were collected by filtration
12. washrinsing forward with hexanes
13. washThe cake was washed with more hexanes
14. customdried on the
15. filtrationfilter