反应详情

温度

65 °C

To a solution of 8-(6-(1-methyl-1H-pyrazol-4-yl)pyridazin-3-yl)-1,4-dioxa-8-azaspiro[4.5]decane, prepared as in STEP 2 above (1.8 g, 6 mmol) in acetone/H2O (30 mL/30 mL) was added p-TSA.H2O (1.37 g, 7.2 mmol). The resulting mixture was stirred at 65° C. for 6 h and then concentrated to remove most of organic solvent. The residue was poured into CH2Cl2/H2O/Na2CO3(aq) (50 mL/25 mL/25 mL). The aqueous layer was extracted with CH2Cl2 (50 mL). The combined organic layer was dried (Na2SO4), and filtered. The solvent was removed by roto-evaporator to yield 1-(6-(1-methyl-1H-pyrazol-4-yl)pyridazin-3-yl)piperidin-4-one as a solid.

1. concentrationconcentrated
2. customto remove most of organic solvent
3. additionThe residue was poured into CH2Cl2/H2O/Na2CO3(aq) (50 mL/25 mL/25 mL)
4. extractionThe aqueous layer was extracted with CH2Cl2 (50 mL)
5. dry with materialThe combined organic layer was dried (Na2SO4)
6. filtrationfiltered
7. customThe solvent was removed by roto-evaporator