反应详情

Through a solution of 3 g (6 mmol) (4-{3-[2-(3,4-Dichloro-phenyl)-2-hydroxy-ethyl]-3-isopropyl-ureido}-benzyl)-carbamic acid tert-butyl ester in 100 mL EtOAc was gently bubbled HCl gas for 15 min. The reaction mixture was then concentrated in vacuo and to the resulting residue was added 15 mL 1N LiOH solution. This was extracted 3×70 ml EtOAc and the combined extracts were washed with 10 ml brine, dried over Na2SO4, filtered and concentrated to give 2.2 g 3-(4-Aminomethyl-phenyl)-1-[2-(3,4-dichloro-phenyl)-2-hydroxy-ethyl]-1-isopropyl-urea as a white solid which was used without further purification. 1H NMR(300 mHz, CD3OD) 7.71 (d, 1H, J=2 Hz); 7.53 (d, 1H, J=8 Hz); 7.37 (dd, 1H, J=8 and 2 Hz); 7.28 (m, 4H); 4.88(m, 1H); 4.34 (sept, 1H, J=7 Hz); 3.78 (s, 2H); 3.48(dd, 1H, J=9 and 16 Hz); 3.22 (m, 2H); 1.25 (d, 3H, J=7 Hz); 1.12 (d, 3H, J=7 Hz).

1. customfor 15 min
2. concentrationThe reaction mixture was then concentrated in vacuo and to the resulting residue
3. additionwas added 15 mL 1N LiOH solution
4. extractionThis was extracted 3×70 ml EtOAc
5. washthe combined extracts were washed with 10 ml brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated