反应详情

To a solution of tert-butyl 2-(4-aminobenzoyl)hydrazinecarboxylate (500 mg, 1.99 mmol) in anhydrous pyridine (10 mL) was added dropwise 3-carbomethoxypropionyl chloride (Fluka) (300 μL) at rt. After 60 min, aminomethyl resin (Polymers Laboratories PL-AMS, 1.96 mmol/g, 400 mg) was added and the resulting mixture was stirred overnight at rt. After filtration and rinsing the resin, water (80 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 70° C. for 2 hrs. The title compound (461 mg) was obtained as a white solid (63%) in 96.0% purity by HPLC (MaxPlot detection between 230 and 400 nm).

1. additionaminomethyl resin (Polymers Laboratories PL-AMS, 1.96 mmol/g, 400 mg) was added
2. filtrationAfter filtration
3. washrinsing the resin, water (80 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 70° C. for 2 hrs