HRID2273027
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
Alternatively, the demethylation can be carried out with LiBr: (3S,11aR)—N-[(2,4-Difluorophenyl)methyl]-3-methyl-6-(methyloxy)-5,7-dioxo-2,3,5,7,11,11a-hexahydro[1,3]oxazolo[3,2-a]pyrido[1,2-d]pyrazine-8-carboxamide (8.609 g) was dissolved in THF (90 mL) and LiBr (3.942 g) was added. The mixture was heated to reflux for 12 h and quenched with H2SO4 (0.5 M, 94.467 g). The resultant suspension was stirred at 20° C. for 2 h and filtered. The solid product was re-slurried in water-THF (50 mL-50 mL) at 20° C. for 2 h. The product was collected by filtration, rinsed with water-THF (1-1, 30 mL), and dried under vacuum to afford the product.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 12 h
- customquenched with H2SO4 (0.5 M, 94.467 g)
- filtrationfiltered
- waitThe solid product was re-slurried in water-THF (50 mL-50 mL) at 20° C. for 2 h
- filtrationThe product was collected by filtration
- washrinsed with water-THF (1-1, 30 mL)
- customdried under vacuum
- customto afford the product