反应详情

To a suspension of 2-amino-1-(6-bromopyridin-2-yl)ethanone hydrochloride (500 mg, 1.99 mmol) obtained in Step 1 of example 6, (S)-N-tert-butylcarbonylalanine (376 mg, 1.99 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (379 mg, 1.99 mmol), 1-hydroxybenzotriazole monohydrate (305 mg, 1.99 mmol) in acetonitrile (11 ml), a solution of triethylamine (0.7 ml) in acetonitrile (4 ml) was added dropwise while ice-cooled for 15 minutes. After the mixture was stirred at the same temperature for 1 hour, water was added and extracted with ethyl acetate. After the organic layer was washed with water, a saturated brine, dried over magnesium sulfate, the residue obtained by vacuum concentration was purified by flash chromatography on silica gel (n-hexane:ethyl acetate=2:1) and the title compound (456 mg, 59%) was obtained.

1. temperaturecooled for 15 minutes
2. extractionextracted with ethyl acetate
3. washAfter the organic layer was washed with water
4. dry with materiala saturated brine, dried over magnesium sulfate
5. customthe residue obtained by vacuum concentration
6. customwas purified by flash chromatography on silica gel (n-hexane:ethyl acetate=2:1)