反应详情

The 3-(tert-butoxycarbonyl)-3-azabicyclo[3.1.0]hexane-6-carboxylic acid (185 mg, 0.812 mmol) prepared in Example 3, hydroxybenzotriazole (132 mg, 0.975 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (187 mg, 0.975 mmol) were dissolved in 3.0 mL of methylene chloride and the (5-isobutyl-3-aminomethyl-1-phenyl)pyrazole (205 mg, 0.894 mmol) prepared in Example 9 was added dropwise. After stirring for 3 hours, the completion of the reaction was confirmed by TLC (hexane:ethyl acetate=1:2). After the reaction was completed, the mixture was extracted with methylene chloride after adding water and saturated sodium bicarbonate. The organic layer was dried with anhydrous sodium sulfate, filtered, concentrated under reduced pressure and separated by column chromatography (hexane:ethyl acetate=1:2) to obtain 328 mg (92.1%) of the target compound.

1. extractionthe mixture was extracted with methylene chloride
2. additionafter adding water and saturated sodium bicarbonate
3. dry with materialThe organic layer was dried with anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customseparated by column chromatography (hexane:ethyl acetate=1:2)