反应详情

3-(2-Methoxy-ethoxy)-5-(pyridine-3-yloxy)-pyridine-2-ylamine (0.48 mmol) is dissolved in THF (7 ml) and 1,1′-thiocarbonyldiimidazole (4 eq.) is added. The reaction solution is stirred 2 days. 32% NH4OH (20 eq.) is added and stirred 4 hours at room temperature. The solved is removed in vacuo and water (150 ml) is added and extracted with dichloromethane. The combined organic layers are washed with brine and dried over MgSO4. The solvent is removed in vacuo. [3-(2-Methoxy-ethoxy)-5-(pyridine-3-yloxy)-pyridine-2-yl]-thiourea is obtained as yellow solid in a yield of 69%. HPLC (method C): 1.15 min; LC-MS (method A): 0.9 min, 321.15 (MH+).

1. stirringstirred 4 hours at room temperature
2. customThe solved is removed in vacuo and water (150 ml)
3. additionis added
4. extractionextracted with dichloromethane
5. washThe combined organic layers are washed with brine
6. dry with materialdried over MgSO4
7. customThe solvent is removed in vacuo