反应详情

5-Methylthiazol-2-amine (5.71 g, 50.0 mmol) and pivaloyl chloride (6.78 mL, 55.0 mmol) were mixed in anhydrous acetonitrile (80 mL) and treated with triethylamine (14.0 mL, 100 mmol) resulting in an exotherm. After 15 minutes, the warm suspension was cooled for 5 minutes with a water bath. The solids were collected by filtration and rinsed with more acetonitrile. The filtrate was partially concentrated and the solids which precipitated were also collected by filtration and rinsed with acetonitrile. The two crops were combined and rinsed with water, and when solids precipitated from the filtrate they were collected by filtration and added to the previously collected material. The crude product was washed with 1:1 dichloromethane/hexanes and dried under vacuum to give the title compound.

1. customresulting in an exotherm
2. temperaturethe warm suspension was cooled for 5 minutes with a water bath
3. filtrationThe solids were collected by filtration
4. washrinsed with more acetonitrile
5. concentrationThe filtrate was partially concentrated
6. customthe solids which precipitated
7. filtrationwere also collected by filtration
8. washrinsed with acetonitrile
9. washrinsed with water, and when solids
10. customprecipitated from the filtrate they
11. filtrationwere collected by filtration
12. additionadded to the previously collected material
13. washThe crude product was washed with 1:1 dichloromethane/hexanes
14. customdried under vacuum