反应详情

To a suspension of 400 mg (1.14 mmol) of potassium 8-(cyclopentylamino)-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate in 80 mL of dichloromethane and a few drops of dimethylformamide 0.11 mL (0.13 mmol) of oxalyl chloride were added at 0° C. The mixture was stirred at room temperature for 6 hours and then evaporated, redissolved in anhydrous dichloromethane and dropped into a solution of 344 mg (2.28 mmol) of N-methylhydroxylamine hydrochloride and 0.33 mL of triethylamine in 20 mL of the same solvent, cooled to 0° C. After 4 hours the mixture was washed with a saturated solution of sodium hydrogenocarbonate, dried over sodium sulfate and evaporated to dryness. The residue was triturated with diethylether and filtered to give 780 mg (60% yield) of the title compound.

1. additionwere added at 0° C
2. customevaporated
3. dissolutionredissolved in anhydrous dichloromethane
4. temperaturecooled to 0° C
5. washAfter 4 hours the mixture was washed with a saturated solution of sodium hydrogenocarbonate
6. dry with materialdried over sodium sulfate
7. customevaporated to dryness
8. customThe residue was triturated with diethylether
9. filtrationfiltered