反应详情

温度

60 °C

To a solution of diethyl(5-bromopyridin-2-yl)malonate (Preparation 84, 5.28 g, 16.70 mmol) in THF (50 mL) was added a solution of LiOH (2.10 g, 50.13 mmol) in water (12.5 mL) and the reaction was heated to 60° C. for 3 hours. The reaction was cooled and acidified to pH 3-4 with 2N HCl and diluted with 20% IPA in DCM. The organic layer was collected, dried over sodium sulphate and concentrated in vacuo. The crude residue was triturated with hexane to afford the title compound.

1. temperatureThe reaction was cooled
2. customThe organic layer was collected
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated in vacuo
5. customThe crude residue was triturated with hexane