反应详情

A solution of 8.20 g (15.77 mmol) of (S)-4-benzyloxy-2-{2-[(2-carboxy-ethyl)-(3,4-dichloro-phenyl)-amino]-ethylamino}-butyric acid methyl ester; HCl in 130 ml CH2Cl2 was treated with 2.20 (15.77 mmol) of triethylamine and at 0° C. with 3.70 g (18.93 mmol) of EDCI. The cooling bath was allowed to come to RT and after 15 h the reaction was extracted with aq. 10% KHSO4/Et2O (3×). The organic phases were washed with aq 10% KHSO4. solution, 10% NaCl and dried over Na2SO4 and purified by flash silica gel column (n-heptane:EtOAc 75:25 to 1:1) to yield 5.64 g (77%) of the title compound as a light yellow oil. MS: 465.1 (MH+, 2Cl).

1. extractionthe reaction was extracted with aq. 10% KHSO4/Et2O (3×)
2. washThe organic phases were washed with aq 10% KHSO4
3. dry with materialsolution, 10% NaCl and dried over Na2SO4
4. custompurified by flash silica gel column (n-heptane:EtOAc 75:25 to 1:1)