反应详情

To a solution of N-{1-[1-(3-methoxypropoxy)-3-methyl-1H-indazol-6-yl]ethyl}-cyclopropanamine (2.63 g) and (2R)-4-(tert-butoxycarbonyl)morpholine-2-carboxylic acid (2.32 g) in N,N-dimethylformamide (25 mL) were added 1-hydroxybenzotriazole (1.36 g) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (2.11 g) under ice-cooling, and then the mixture was stirred at room temperature for 3 hours. To the reaction mixture was added ethyl acetate, and the mixture was washed with saturated saline, dried over magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate/methanol=30/3/1→9/3/1) to give tert-butyl (2R)-2-[(cyclopropyl{(1R)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}amino) carbonyl]morpholin-4-carboxylate [Ex(162-1)] (1.71 g) and tert-butyl (2R)-2-[(cyclopropyl{(1S)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}amino) carbonyl]morpholin-4-carboxylate [Ex(162-1)] (468 mg) as a colorless oil.

1. temperaturecooling
2. washthe mixture was washed with saturated saline
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate/methanol=30/3/1→9/3/1)