反应详情

To a solution of tert-butyl 2-(4-aminobenzoyl)hydrazinecarboxylate (1.0 g, 3.98 mmol) in anhydrous pyridine (20 mL) was added dropwise methyl 6-chloro-6-oxohexanoate (Fluka) (750 μL) at rt. After 30 min, aminomethyl resin (Polymers Laboratories PL-AMS, 1.96 mmol/g, 970 mg) was added and the resulting mixture was stirred overnight at rt. After filtration and rinsing the resin, water (160 mL) was added into the filtrate and a white solid precipitated out. Filtration and washing with water gave a white solid, which was dried under vacuo at 50° C. for 5 hrs. The title compound (981 mg) was obtained as a white solid (63%) in 99.8% purity by HPLC (MaxPlot detection between 230 and 400 nm).

1. additionaminomethyl resin (Polymers Laboratories PL-AMS, 1.96 mmol/g, 970 mg) was added
2. filtrationAfter filtration
3. washrinsing the resin, water (160 mL)
4. additionwas added into the filtrate
5. customa white solid precipitated out
6. filtrationFiltration
7. washwashing with water
8. customgave a white solid, which
9. customwas dried under vacuo at 50° C. for 5 hrs