HRID2273027

反应详情

EQUATION

反应方程式

HRID 2273027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 12 h
  3. customquenched with H2SO4 (0.5 M, 94.467 g)
  4. filtrationfiltered
  5. waitThe solid product was re-slurried in water-THF (50 mL-50 mL) at 20° C. for 2 h
  6. filtrationThe product was collected by filtration
  7. washrinsed with water-THF (1-1, 30 mL)
  8. customdried under vacuum
  9. customto afford the product