反应详情

To a mixture of 2-hydroxymethyl-5-propoxy-pyridin-4-ol (5.56 g, 30.3 mmole) and 30 mL of chloroform stirred cooled with an ice bath is added 30 mL of thionyl chloride (x g, 0.x mole). This is stirred for 15 minutes at ice bath temperature and then refluxed for 1 hour. The reaction mixture is cooled, evaporated to dryness in vacuo and then treated with isopropanol. The solid is filtered, washed with fresh isopropanol, then ether and air dried to give an off-white solid, 3.4 g, (48%), m.p. 165-7° C.; MS (ES+): m/z 202.3 (M+H).

1. temperaturecooled with an ice bath
2. stirringThis is stirred for 15 minutes at ice bath temperature
3. temperaturerefluxed for 1 hour
4. temperatureThe reaction mixture is cooled
5. customevaporated to dryness in vacuo
6. additiontreated with isopropanol
7. filtrationThe solid is filtered
8. washwashed with fresh isopropanol
9. dry with materialether and air dried
10. customto give an off-white solid, 3.4 g, (48%), m.p. 165-7° C.