反应详情

温度

0 °C

Trifluoroacetic acid (10 mL) was added slowly to a cooled (0° C.) solution of N′-(2-fluoro-phenyl)-N′-((1S,4S)-4,7,7-trimethyl-3-oxo-bicyclo[2.2.1]heptane-2-carbonyl)-hydrazinecarboxylic acid tert-butyl ester (˜5.3 mmol) in dichloromethane (10 mL), and the resulting solution was stirred at 0° C. for 10 min and then at room temperature for 3.5 h. The solvent was evaporated and dichloromethane (80 mL) was added. The solution was washed with water (4×20 mL) and brine (20 mL), dried (magnesium sulfate), filtered, and evaporated to give an orange foam. This was triturated with 10% ethyl acetate/hexane (25 mL) and the mixture was cooled in an ice-bath at 0° C. for 1 h. The solid was filtered off and dried to give (4R,7S)-2-(2-fluoro-phenyl)-7,8,8-trimethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (890 mg, 58%) as a pale yellow solid.

1. waitat room temperature for 3.5 h
2. customThe solvent was evaporated
3. additiondichloromethane (80 mL) was added
4. washThe solution was washed with water (4×20 mL) and brine (20 mL)
5. dry with materialdried (magnesium sulfate)
6. filtrationfiltered
7. customevaporated
8. customto give an orange foam
9. customThis was triturated with 10% ethyl acetate/hexane (25 mL)
10. temperaturethe mixture was cooled in an ice-bath at 0° C. for 1 h
11. filtrationThe solid was filtered off
12. customdried