反应详情

温度

0 °C

To a suspension of the oxime from Step 3 (2.0 g, 5.9 mmol) in ethanol (35 mL) at 0° C. there was added pyridine-borane (1.1 g, 11.8 mmol) and 12 N aqueous HCl (1.48 mL, 17.75 mmol). The mixture was stirred at 0° C. for 1 hour, then warmed to room temperature. Most of the ethanol was evaporated, the residue was diluted with water and ethyl acetate (the product as hydrochloride salt remains in the organic phase) and was basified with 1N aqueous NaOH. The product obtained from the organic phase was triturated with hexane and was filtered to afford the title compound as a yellow solid, mp: 126° C. dec.

1. temperaturewarmed to room temperature
2. customMost of the ethanol was evaporated
3. additionthe residue was diluted with water and ethyl acetate (the product as hydrochloride salt
4. customThe product obtained from the organic phase
5. customwas triturated with hexane
6. filtrationwas filtered