反应详情

The solution of methyl 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboximidate in methanol obtained from Example 5A is mixed with 33.76 g (32.19 ml, 562 mmol) of glacial acetic acid and 9.28 g (173 mmol) of ammonium chloride and stirred under reflux overnight. The solvent is evaporated in vacuo, the residue is thoroughly triturated with acetone, and the precipitated solid is filtered off with suction. It is added to 2 l of water, 31.8 g of sodium carbonate are added while stirring, the mixture is extracted three times with a total of 1 l of ethyl acetate, and the organic phase is dried with magnesium sulphate and evaporated in vacuo.

1. temperatureunder reflux overnight
2. customThe solvent is evaporated in vacuo
3. customthe residue is thoroughly triturated with acetone
4. filtrationthe precipitated solid is filtered off with suction
5. additionIt is added to 2 l of water, 31.8 g of sodium carbonate
6. additionare added
7. stirringwhile stirring
8. extractionthe mixture is extracted three times with a total of 1 l of ethyl acetate
9. dry with materialthe organic phase is dried with magnesium sulphate
10. customevaporated in vacuo