反应详情

A solution of ethyl (3R,4S)-4-{[(4-chloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-propoxypiperidine-1-carboxylate (Intermediate 73, 2.8 g, 7.547 mmol) potassium hydroxide (4.2 g, 75.47 mmol), and Hydrazine hydrate (3.6 mL, 75.47 mmol) in ethylene glycol (100 mL) was stirred for 60 h at 120° C. The reaction mixture was poured into water (300 mL) and extracted with ethyl acetate (2×300 mL). The combined organic extracts were dried over anhydrous sodium sulphate, filtered, and concentrated under vacuum to afford 4-chloro-5-methyl-N-[(3S,4R)-3-propoxypiperidin-4-yl]-1H-pyrrole-2-carboxamide 650 mg, 30% as solid.

1. extractionextracted with ethyl acetate (2×300 mL)
2. dry with materialThe combined organic extracts were dried over anhydrous sodium sulphate
3. filtrationfiltered
4. concentrationconcentrated under vacuum