反应详情

温度

50 °C

Following the procedure of Harada et al., Heterocycles 1998, 48, 695-702, to a solution of 5-(5-amino-2-isopropyl-4-methoxy-phenoxy)-pyrimidine-2,4-diamine (0.400 g, 1.8 mmol) in 5 ml methanol at 0° C. was added trimethylamime (0.308 g, 3.0 mmol) and hydrazine 1,1-dichloroethyl hydrazine tosylate (0.388 g, 1.4 mmol). The solution was warmed to 50° C. After 4 h the mixture was concentrated in vacuo and extracted with CH2Cl2. The combined organics were washed with H2O, washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo. Purification via flash chromatography (94:6 CH2Cl2/MeOH) afforded 5-(2-isopropyl-4-methoxy-5-[1,2,3]triazol-1-yl-phenoxy)-pyrimidine-2,4-diamine (0.145 g, 31%) as a white solid; [MH]+=342.

1. concentrationAfter 4 h the mixture was concentrated in vacuo
2. extractionextracted with CH2Cl2
3. washThe combined organics were washed with H2O
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification via flash chromatography (94:6 CH2Cl2/MeOH)