反应详情

温度

20 °C

A solution of 3-isothiocyanatopyridine (1.36 g) in absolute ethanol (40 cc) is added dropwise, at a temperature of about 0° C., to a solution of (RS)-5-hydroxymethyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine (1.69 g) in absolute ethanol (60 cc). The resulting solution is stirred for 20 hours at a temperature of about 20° C. and the solid formed is then filtered off. The filtrate is evaporated to dryness under reduced pressure (25 mm Hg; 3.3 kPa) at 40° C. and a white solid is obtained which is combined with the solid isolated by filtration. These solids are dissolved in a mixture, heated under reflux, of isopropanol and diisopropyl ether (1:2 by volume; 150 cc) and the solution, after cooling, is kept at +5° C. for 20 hours. The resulting crystals are filtered off, washed with diisopropyl ether (50 cc) and dried at 20° C. under reduced pressure (0.1 mm Hg; 0.013 kPa). (RS)-5-Hydroxymethyl-6-[(pyrid-3-yl)thiocarbamoyl]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine (2.3 g) is thus obtained in the form of white crystals melting at 165° C.

1. customthe solid formed
2. filtrationis then filtered off
3. customThe filtrate is evaporated to dryness under reduced pressure (25 mm Hg; 3.3 kPa) at 40° C.
4. customa white solid is obtained which
5. customisolated by filtration
6. dissolutionThese solids are dissolved in a mixture
7. temperatureheated
8. temperaturethe solution, after cooling
9. waitis kept at +5° C. for 20 hours
10. filtrationThe resulting crystals are filtered off
11. washwashed with diisopropyl ether (50 cc)
12. customdried at 20° C. under reduced pressure (0.1 mm Hg; 0.013 kPa)