反应详情

To a solution of compound B (103.0 g, 340.7 mmol) in MeOH (1200 ml) was added a solution of LiOH (16.4 g, 681.4 mmol) in water (120 ml). The reaction mixture was stirred at room temperature for 3 h. Solvents were evaporated to ¾ of initial volume followed by dilution with water (400 ml). Solution was extracted with EtOAc (2×300 ml). The organic layer was washed with brine (200 ml), dried over MgSO4 and evaporated in vacuo. The resultant residue was dissolved in ether (300 ml) and treated with 2 N HCl/ether (200 ml). The formed precipitate was filtered, washed with ether and dried in vacuo to provide hydrochloric salt of compound C (54.5 g, 261.2 mmol) as white solid. LC-MS [M+H] 209.5 (C11H16N2O2+H, calc: 209.3).

1. customSolvents were evaporated
2. extractionSolution was extracted with EtOAc (2×300 ml)
3. washThe organic layer was washed with brine (200 ml)
4. dry with materialdried over MgSO4
5. customevaporated in vacuo
6. dissolutionThe resultant residue was dissolved in ether (300 ml)
7. additiontreated with 2 N HCl/ether (200 ml)
8. filtrationThe formed precipitate was filtered
9. washwashed with ether
10. customdried in vacuo