反应详情

Combine 5-benzyloxytryptamine hydrochloride (1 g, 3.3 mmol), phthalic anhydride (.56 g, 4.0 mmol) and N,N-diisopropylethylamine (0.86 g, 6.6 mmol) in 25 mL anhydrous pyridine and reflux for 1 hour, cool to room temperature and treat with 4 g 3 Å molecular sieves. Refluxing was continued for 60 hours then the mixture was filtered. Concentrate under vacuum to give a residue which is mixed with 25 mL CHCl3 and filtered to give a solid. Purification of the filtrate by chromatography on silica gel eluting with 1% MeOH in CHCl3 to give an additional amount of title compound: ISMS 397 (M+1); Analysis for C25H20N2O3 0.3H2O C7H8: calcd: C, 75.09; H, 5.25; N, 6.82; found: C, 75.00; H, 5.22; N, 6.96.

1. additiontreat with 4 g 3 Å molecular sieves
2. temperatureRefluxing
3. filtrationthe mixture was filtered
4. concentrationConcentrate under vacuum
5. customto give a residue which
6. filtrationfiltered
7. customto give a solid
8. customPurification of the filtrate by chromatography on silica gel eluting with 1% MeOH in CHCl3