反应详情

温度

0 °C

A solution of 7.76 g (21.43 mmol) of 3-[(3,4-dichloro-phenyl)-methoxycarbonylmethyl-amino]-propionic acid tert-butyl ester in 250 ml of ETOH was treated at 0° C. with 0.98 g (42.86 mmol) of LiBH4. The reaction was stirred 10 min at 0° C. and 15 h at RT. After cooling (0° C.) a second batch of 0.49 g (21.43 mmol) of LiBH4 was added and stirred 6 h at RT. The reaction was cooled (0° C.), neutralized with aq. 10% KHSO4 solution and extracted with EtOAc (3×). The organic phase was dried over Na2SO4 evaporated and purified by flash silica gel column (n-heptane:EtOAc 9:1 to 1:1) to yield 6.12 g (85%) of the title compound as light yellow oil. MS: 334.2 (MH+, 2Cl).

1. additionwas added
2. stirringstirred 6 h at RT
3. temperatureThe reaction was cooled (0° C.)
4. extractionextracted with EtOAc (3×)
5. dry with materialThe organic phase was dried over Na2SO4
6. customevaporated
7. custompurified by flash silica gel column (n-heptane:EtOAc 9:1 to 1:1)