反应详情

温度

0 °C

A solution of 0.50 g (1.3 mmol) of 3-[(3-chloro-4-trifluoromethoxy-phenyl)-(2-oxo-ethyl)-amino]-propionic acid tert-butyl ester in 6 ml dichloromethane was added dropewise to a cooled (0° C., pH ca. 5) suspension of 0.22 g (1.4 mmol) methyl 4-aminobutyrate hydrochloride, 0.18 ml (1.3 mmol) triethylamine, 0.15 ml (2.6 mmol) acetic acid and 0.32 g (1.5 mmol) sodium triacetoxyborohydride in 4 ml of dichloromethane and stirred 30 min at 0° C. The reaction was extracted with aqueous saturated NaHCO3/EtOAc (3×). The organic phases were washed with aqueous saturated NaHCO3 and dried over Na2SO4 to yield after evaporation of the solvent 0.61 g (83%) of the titled compound as yellow oil. MS: 483.19 (MH+, Cl).

1. temperaturea cooled
2. extractionThe reaction was extracted with aqueous saturated NaHCO3/EtOAc (3×)
3. washThe organic phases were washed with aqueous saturated NaHCO3
4. dry with materialdried over Na2SO4
5. customto yield
6. customafter evaporation of the solvent 0.61 g (83%) of the titled compound as yellow oil