反应详情

A solution of 9.61 g (59.33 mmol) of 3,4-dichloro-phenylamine and 10.21 ml (59.33 mmol) of 2,6-lutidine in 55 ml of toluene was treated slowly with 6.50 ml (59.33 mmol) of tert-butyl 3-bromopropionate and stirred 30 h at reflux temperature. The reaction was then partitioned between 10% aq. KHSO4 solution and EtOAc (3×). The organic phases were washed with 10% aq. NaCl solution, dried over Na2SO4 evaporated and purified by flash silica gel column (n-heptane:EtOAc 9:1) to yield 8.98 g (52%) of the title compound as off-white solid. MS: 290.0 (MH+, 2Cl).

1. temperatureat reflux temperature
2. customThe reaction was then partitioned between 10% aq. KHSO4 solution and EtOAc (3×)
3. washThe organic phases were washed with 10% aq. NaCl solution
4. dry with materialdried over Na2SO4
5. customevaporated
6. custompurified by flash silica gel column (n-heptane:EtOAc 9:1)