反应详情

温度

80 °C

A mixture of 6-methyl-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine (6.3 g; 41 mmoles), p-nitro-phenol (5.7 g; 41 mmoles), polyoxymethylene (2.5 g; 83 mmoles) and dioxan (50 cc) is stirred at 80° C. during 4 hours. After concentration in vacuo, the residue is dissolved in ether and then treated with 0.5 equivalent oxalic acid in ethanol solution. The resulting semi-oxalate is filtered, washed with boiling methanol-water (1:3), filtered again and dried (M.p.= 214° C.; yield: 27%).

1. concentrationAfter concentration in vacuo
2. dissolutionthe residue is dissolved in ether
3. filtrationThe resulting semi-oxalate is filtered
4. washwashed with boiling methanol-water (1:3)
5. filtrationfiltered again
6. customdried (M.p.= 214° C.; yield: 27%)