反应详情

Thionyl chloride (6.25 g, 0.052 mole) was added dropwise to a stirred solution of 2-hydroxymethyl-4-phenylthiazole (9.55 g; 0.05 mole) and dry pyridine (4.0 g; 0.051 mole) in dry benzene (60 ml) held at room temperature. The mixture was stirred and heated to boiling for 1 hour. The cooled reaction mixture was then shaken with 2 × 70 ml H2O and dried over anhydrous MgSO4. The solvent was removed under vacuum and the remaining red oil extracted with 40°-60° C. petroleum ether (100 ml), discarding a small tarry residue. The extract was treated with decolourising charcoal, filtered and evaporated, leaving a yellow-red oil that crystallised on refrigeration.

1. customheld at room temperature
2. temperatureheated
3. customThe cooled reaction mixture
4. dry with materialdried over anhydrous MgSO4
5. customThe solvent was removed under vacuum
6. extractionthe remaining red oil extracted with 40°-60° C. petroleum ether (100 ml)
7. additionThe extract was treated with decolourising charcoal
8. filtrationfiltered
9. customevaporated
10. customleaving a yellow-red oil that
11. customcrystallised on refrigeration