反应详情

270 g of the nitro derivative (a) is added to 1.570 liters of ethanol and 21 g of Raney nickel in an autoclave. Hydrogen is added under a pressure of 10 atmospheres and the reactants are heated at a temperature of 65° while stirring. After 1 hour 45 minutes the theoretical volume of hydrogen has been absorbed. The solution is cooled and filtered. The ethanol is distilled in vacuo, the residue is dissolved in 0.6 l of methanol, 60 g of potassium hydroxide tablets are added, and the mixture is heated under reflux for 1 hour while stirring. The mixture is cooled and allowed to crystallise. 194.5 g (yield=76%) of 2-methyl-6,7,8-trimethoxy-1-(4,5,6-triethoxy-7-amino-3-phthalidyl)-1,2,3,4-tetrahydro-isoquinoline is obtained in the form of white crystals having a melting point of 144° and exhibiting only a single spot when analysed by thin layer chromatography.

1. temperaturethe reactants are heated at a temperature of 65°
2. customAfter 1 hour 45 minutes the theoretical volume of hydrogen has been absorbed
3. temperatureThe solution is cooled
4. filtrationfiltered
5. distillationThe ethanol is distilled in vacuo
6. dissolutionthe residue is dissolved in 0.6 l of methanol
7. addition60 g of potassium hydroxide tablets are added
8. temperaturethe mixture is heated
9. temperatureunder reflux for 1 hour
10. stirringwhile stirring
11. temperatureThe mixture is cooled
12. customto crystallise