反応 #76485

反応方程式

product

8-Bromo-1,2,3,4-tetrahydro-2-methyl-5,6-isoquinolinediamine

oxalic acid

→

title compound

収率 24.1%

6-Bromo-1,4,7,8,9,10-hexahydro-8-methylpyrido[4,3-f]-quinoxaline-2,3-dione

収率 24.1%

溶媒

HCl

反応条件

後処理

1. 1
   温度at reflux for 18 hours
2. 2
   その他the solid which formed
3. 3
   ろ過was collected by filtration
4. 4
   洗浄washed with cold water
5. 5
   その他The solid was recrystallized from hot water
6. 6
   乾燥dried under vacuum (100° C., P2O5)

実験手順

A solution of the product from Example 13 (0.62 g, 2.56 mmol) and oxalic acid (0.23 g, 2.56 mmol) in 25 mL of 3N aqueous HCl solution were heated at reflux for 18 hours. The reaction mixture was cooled to room temperature and the solid which formed was collected by filtration and washed with cold water. The solid was recrystallized from hot water and dried under vacuum (100° C., P2O5) to give the title compound as a tan solid (0.191 g, 20%), mp=315-320° C. (dec.).

出典