反应详情

A solution of ethyl (3S,4R)-4-{[(4-chloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-ethoxypiperidine-1-carboxylate (Intermediate 34, 1.6 g, 4.48 mmol), potassium hydroxide (1.76 g, 31.37 mmol), and hydrazine hydrate (1.6 mL, 31.37 mmol) in ethylene glycol (180 mL) was stirred for 40 h at 120° C. The reaction mixture was poured in to water (120 mL) and extracted with ethyl acetate (2×150 mL). The combined organic extracts were dried over anhydrous sodium sulphate, filtered, concentrated in vacuo to yield the crude product which was triturated with water (30 mL) to afford 4-chloro-N-[(3S,4R)-3-ethoxypiperidin-4-yl]-5-methyl-1H-pyrrole-2-carboxamide 480 mg (37%) as solid.

1. extractionextracted with ethyl acetate (2×150 mL)
2. dry with materialThe combined organic extracts were dried over anhydrous sodium sulphate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customto yield the crude product which
6. customwas triturated with water (30 mL)