反应详情

温度

4 °C

To a cooled solution of thionylchloride (41 ml, 344 mmol) at 0° C. was added cautiously (highly exothermic) portionwise (5-bromo-pyridin-3-yl)-methanol (10 g, 44.5 mmol). After complete addition the mixture was heated to reflux for 1 h to complete the reaction. After cooling, ether (50 ml) was added and the mixture cooled to 4° C. The precipitated solid was filtered off and washed with cold ether then dried at 50° C. under vacuum for 2 h to afford the title compound (9.1 g, 84%) as a light yellow solid. MS: m/e=206.9 (M+).

1. additionAfter complete addition the mixture
2. temperaturewas heated
3. temperatureto reflux for 1 h
4. customthe reaction
5. temperatureAfter cooling
6. filtrationThe precipitated solid was filtered off
7. washwashed with cold ether
8. customthen dried at 50° C. under vacuum for 2 h