反应详情

In a 3-neck round bottom flask mix 2-amino-5-methyl-thiazole-4-carboxylic acid ethyl ester (62.9 g, 338 mmol) and THF (630 mL). Heat to reflux and treat the reaction mixture with isoamyl nitrile (52.6 g, 60.1 mL, 449 mmol) dropwise. Upon completion of the addition, stir the reaction at reflux for 1 h, then concentrate the reaction mixture by rotavap (hi-vac) to give 70 g crude product as a thick orange oil. Purify on silica gel (400 g, 20-45% EtOAc/hexanes) to afford 39.47 g (68%) of the title compound as a yellow solid. LC-ES/MS m/z 172 (M+1), TR=1.5 min.

1. temperatureHeat
2. temperatureto reflux
3. additionUpon completion of the addition
4. customthe reaction
5. temperatureat reflux for 1 h
6. concentrationconcentrate the reaction mixture by rotavap (hi-vac)
7. customto give 70 g crude product as a thick orange oil
8. customPurify on silica gel (400 g, 20-45% EtOAc/hexanes)