反应详情

Methyl4-[(9-cyclopentyl-5-methyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-yl)amino]-3-methoxybenzoate (Intermediate 7; 250 mg, 0.61 mmol) and HCl (2 mL, concentrated aqueous) were suspended in water (4 mL) and heated at reflux for 24 h. The reaction mixture was then cooled to ambient temperature and the volatiles were removed under reduced pressure. The solid obtained was dissolved in MeOH:DCM (1:10, 40 mL) and washed with NaHCO3 (saturated aqueous, 40 mL). The organic layer was then dried (MgSO4), filtered and the volatiles removed under reduced pressure to afford the title compound (240 mg, 99%) as a solid.

1. temperatureheated
2. temperatureat reflux for 24 h
3. customthe volatiles were removed under reduced pressure
4. customThe solid obtained
5. washwashed with NaHCO3 (saturated aqueous, 40 mL)
6. dry with materialThe organic layer was then dried (MgSO4)
7. filtrationfiltered
8. customthe volatiles removed under reduced pressure