反应详情

温度

0 °C

A solution of 2,2-dimethyl-N-(6-methyl-pyridazin-3-yl)-propionamide (4.00 g, 20.73 mmol) in THF (50 mL) is stirred at 0° C. 2.0 M iPrMgBr (46.6 mL, 93.26 mmol) is then added dropwise. The reaction is stirred at 0° C. for 30 min, then it is refluxed for 2 h. It is cooled to rt, poured into ice-H2O; sat. NH4Cl is added and extracted with EtOAc; dried with Na2SO4, filtered and concentrated. The crude material is dissolved in CH2Cl2 (100 mL), treated with 12 (5.8 g, 22.80 mmol) and stirred at rt for 2 h. The reaction is diluted with CH2Cl2 (100 mL), washed with 5% Na2SO3 (3×100 mL); dried with Na2SO4, filtered and concentrated. Purification of the crude material gives the title compound (1.38 g, 5.87 mmol, 28%). ES-MS (m/z): calcd for C13H21N3O (M+H)+: 236.3. found: 236.1.

1. temperatureit is refluxed for 2 h
2. temperatureIt is cooled to rt
3. extractionextracted with EtOAc
4. dry with materialdried with Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. dissolutionThe crude material is dissolved in CH2Cl2 (100 mL)
8. stirringstirred at rt for 2 h
9. washwashed with 5% Na2SO3 (3×100 mL)
10. dry with materialdried with Na2SO4
11. filtrationfiltered
12. concentrationconcentrated
13. customPurification of the crude material