反应详情

温度

0 °C

6.1 g (153 mmol, 60% w/w in mineral oil) NaH were dissolved in THF (90 ml) at 0° C. At this temperature 3.4 g (54.7 mmol) ethane thiol were added. After stirring for 15 min at 0° C., 12.4 g (60.2 mmol) 2,6-dichloro-4-methyl-pyridine-3-carboxylic acid were added portionwise. The RM was allowed to warm to RT and stirring was continued at RT for 16 h. Then the reaction was quenched with a 2M aq. HCl and diluted with EtOAc. The organic layer was separated, dried over MgSO4 and concentrated in vacuo. Crystallisation (DCM/hexane) of the residue yielded 12.0 g (51.7 mmol, 95%) 6-chloro-2-ethylsulfanyl-4-methyl-pyridine-3-carboxylic acid.

1. temperatureto warm to RT
2. stirringstirring
3. waitwas continued at RT for 16 h
4. customThen the reaction was quenched with a 2M aq. HCl
5. additiondiluted with EtOAc
6. customThe organic layer was separated
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo
9. customCrystallisation (DCM/hexane) of the residue