反应详情

温度

100 °C

To a solution of 5-bromo-2-ethyl-pyridin-3-ylamine (1.492 mmol), synthesized in a similar manner as described for 5-bromo-2-methyl-pyridin-3-ylamine (Stage 75.1.4) using diethyl methylmalonate (HPLC: tR 1.71min (Method A); M+H=201, 203 MS-ES), in chloroform (0.75 ml) and 2-methoxypropene (Aldrich, Buchs, Switzerland, 7.46 mmol) were added triethylamine (1.492 mmol) and pyridinium para-toluensulfonate (0.149 mmol). The RM was stirred for 17 h at 100° C., then was quenched with aqueous Na2CO3 and extracted with EtOAc (2×). The combined organic layers were washed with brine, dried over Na2SO4, filtered, evaporated and dried under vacuum to give the title compound as a brown oil (M+H=241, 243 MS-ES).

1. customwas quenched with aqueous Na2CO3
2. extractionextracted with EtOAc (2×)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customevaporated
7. customdried under vacuum