反应详情

温度

90 °C

Oxalyl chloride (42.0 mL, 481 mmol) was dissolved in anhydrous 1,4-dioxane (400 mL) under an N2 atmosphere. The resulting solution was heated to 90° C. To the hot solution was slowly added a solution of 2-amino-4,6-bis(2,2,2-trifluoroethoxy)pyrimidine (14.0 g, 48 mmol) in anhydrous 1,4-dioxane (50 mL). After addition of the aminopyrimidine solution was complete, heating was continued for 6 h, the heat removed, and the solution cooled to room temperature. The solution was concentrated and the residue distilled at reduced pressure to afford the product as a clear oil (12.4 g, 82% yield): by 53-54° C. (ca. 0.1 to 0.2 mm Hg): 1H NMR (CDCl3) δ 6.19 (s, 1H), 4.82-4.74 (q, 2H, J=8.2 Hz).

1. temperatureheating
2. customthe heat removed
3. temperaturethe solution cooled to room temperature
4. concentrationThe solution was concentrated
5. distillationthe residue distilled at reduced pressure