反应详情

温度

65 °C

To a solution of 4-(4-chloro-6-thiophen-3-yl-[1,3,5]triazin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (169 mg, 0.29 mmol) in 2-propanol/EtOAc (10:1, 11 mL) at room temperature was added DIEA (0.5 mL). The resulting solution was vacuum-flushed with N2 and then treated with 10% Pd/C (50 mg). The resulting suspension was exposed to H2 via balloon and heated to 65° C. After 3 h, 10% Pd/C (50 mg) was added, and the reaction mixture was heated at 65° C. overnight under H2. The resulting mixture was filtered to remove catalyst; the filtrate was concentrated and the residue was purified by preparative TLC (EtOAc/hexanes, 1:2) to yield a white solid.

1. customThe resulting solution was vacuum-flushed with N2
2. additiontreated with 10% Pd/C (50 mg)
3. addition10% Pd/C (50 mg) was added
4. temperaturethe reaction mixture was heated at 65° C. overnight under H2
5. filtrationThe resulting mixture was filtered
6. customto remove catalyst
7. concentrationthe filtrate was concentrated
8. customthe residue was purified by preparative TLC (EtOAc/hexanes, 1:2)
9. customto yield a white solid