Yield:52319-97-8 82%

Reaction Conditions:

with ammonia;sodium methylate in methanol; for 6 h;Heating / reflux;

Steps:

1.i

i) 4-Tert-butyldiiminoisoindoline 1 4-Tert-butylphthalonitrile (1.5 g, 8.14 mmol) was added to dry MeOH (300 mL) and the mixture was stirred until it was dissolved. After confirmation of complete dissolution, NH₃ gas was introduced for 15 minutes. NaOMe (34 mg, 0.63 mmol) suspended in 10 mL of dry MeOH was added to the reaction solution, and NH₃ gas was introduced repeatedly for 10 minutes at intervals of 20 minutes, while the reaction solution was refluxed under heating. Six hours after initiation of the reaction, disappearance of the raw materials was confirmed by TLC, and the reaction solution was cooled to room temperature and MeOH was evaporated. The residual pale-blue powdery compound was washed with cold water, to give a colorless solid. Yield: 1.34 g, 82%

References:

EP1690865,2006,A1 Location in patent:Page/Page column 12