反应详情

Add bromine (195; mL, 3.81; mol) over 10; min to a heated solution of 2-cyano-3-oxo-thiobutyramide (550; g, 3.86; mol) in glacial acetic acid (5.80; L) at 40° C. and stir at room temperature for 15; h. Filter the reaction mixture, wash the collected solid with water and dry overnight under vacuum to give a dark red solid (1151; g). Slurry the solid with stirring in a saturated aqueous solution of sodium bicarbonate (8; L) for 30; min and filter. Wash the collected solid with water and dry overnight under vacuum to give a dark red solid (1022; g). Slurry the solid with stirring with methyl t-butyl ether (5.90; L) over 1 hour, filter and retain the filtrate. Repeat the above methyl t-butyl ether extraction process twice on recovered solid retaining the filtrate after each extraction. Combine the filtrates and concentrate to give the title compound as a yellow solid which is carried on without further purification (598; g, 72%). MS (m/z): 221, 223; (M+1).

1. filtrationFilter the reaction mixture
2. washwash the collected solid with water
3. customdry overnight under vacuum
4. customto give a dark red solid (1151; g)
5. filtrationmin and filter
6. washWash the collected solid with water
7. customdry overnight under vacuum
8. customto give a dark red solid (1022; g)
9. filtrationfilter
10. extractionRepeat the above methyl t-butyl ether extraction process twice
11. customon recovered solid
12. extractionafter each extraction
13. concentrationconcentrate