反应详情

5-Carboxyphthalid (36 g, 0.2 mole) is suspended in thionylchloride (100 mL). DMF (1.5 mL) is added and the mixture is refluxed for 1 hour. Toluene (200 mL) is added and the solvents are evaporated in vacuo. The residue is dissolved in THF (200 mL) and added to a solution of tert.butylamine (31 g, 0.42 mole) in THF (200 mL) at 5° C. The mixture is allowed to warm to room temperature and stirred overnight. The reaction is then poured into ice water (400 mL) and the precipitated crystals are filtered off. The crystals are washed with water (100 mL). Yield: 41 g, 87%. DSC onset: 189.5° C.

1. temperaturethe mixture is refluxed for 1 hour
2. customthe solvents are evaporated in vacuo
3. dissolutionThe residue is dissolved in THF (200 mL)
4. filtrationthe precipitated crystals are filtered off
5. washThe crystals are washed with water (100 mL)
6. custom189.5° C.