反应详情

温度

0 °C

To a solution of 3-bromo-4-methoxy-N2-phenylbenzene-1,2-diamine (421 mg, 1.8 mmol), Boc-ala-OH (343 mg, 1.8 mmol) and HOAT (247 mg, 1.8 mmol) in DCM (10 mL) at 0° C. was added N-(3-dimethylaminopropyl)-n′-ethylcarbodiimide hydrochloride (383 mg, 1.99 mmol) and the reaction mixture stirred at 0° C. for 1 h. The reaction mixture was diluted with water and extracted with DCM (3×10 mL). The combined organic fractions were washed with brine, dried (MgSO4) and concentrated in vacuo. The residue was dissolved in HCl in dioxane (10 mL, 4 M) and the reaction mixture heated at 75° C. for 1 h. The reaction mixture was concentrated in vacuo to give the title product as a dark purple solid (758 mg, 100%). LCMS (Method C): RT=2.15 min, [M+H]+=346 & 348.

1. extractionextracted with DCM (3×10 mL)
2. washThe combined organic fractions were washed with brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. dissolutionThe residue was dissolved in HCl in dioxane (10 mL, 4 M)
6. temperaturethe reaction mixture heated at 75° C. for 1 h
7. concentrationThe reaction mixture was concentrated in vacuo