反应详情

温度

45 °C

To a solution of 1-tert-butoxy-3-fluoro-5-isothiocyanatobenzene (460 g, 2.04 mol) in anhydrous isopropyl alcohol (3250 ml) was added triethylamine (315 g, 3.06 mol). The mixture was heated to reflux under N2 atmosphere for 16 h and the temperature was cooled to 40-50° C. After concentration, the resulting dark residue was diluted with n-heptane (1000 ml) and heated to 60° C. The mixture was slowly cooled to 25° C., at the same time seeding was added. A slurry was observed and stirred at 25° C. for 16 h before being cooled slowly to 0-10° C. within 2 h. After filtration and washing with n-heptane (200 ml), the collected solid was dried in oven under vacuum at 40-45° C. for 18 h to give (3-tert-Butoxy-5-fluoro-phenyl)-thiocarbamic acid O-isopropyl ester (453.1 g).

1. temperatureThe mixture was heated
2. temperatureto reflux under N2 atmosphere for 16 h
3. concentrationAfter concentration
4. additionthe resulting dark residue was diluted with n-heptane (1000 ml)
5. temperatureheated to 60° C
6. temperatureThe mixture was slowly cooled to 25° C., at the same time seeding
7. additionwas added
8. temperaturebefore being cooled slowly to 0-10° C. within 2 h
9. filtrationAfter filtration
10. washwashing with n-heptane (200 ml)
11. customthe collected solid was dried in oven under vacuum at 40-45° C. for 18 h