Potassium Carbonate → HCID 178486249, compound

Participants

Reaction Steps

21 mg (154 μmol) of potassium carbonate are added to a solution of 0.09 g (154 μmol) of tert-butyl 5-(N′-methyl-N′-phenylhydrazinocarbonyl)-3-(4-morpholin-4-ylmethylbenzoylamino)thieno[2,3-c]pyrazole-1-carboxylate in 5 mL of methanol in a microwave oven tube. The tube is stoppered and the reaction mixture is irradiated at a temperature in the region of 180° C. for 3 minutes. The reaction mixture is then concentrated to dryness under vacuum (0.6 kPa) at a temperature in the region of 30° C. The residue is purified by chromatography on a cartridge of 25 g of silica gel (0.015-0.040 mm), eluting with a dichloromethane/methanol mixture (99/1 by volume, then 98/2 and finally 97/3) at a flow rate of 10 mL/min. The fractions containing the expected product are combined and then concentrated to dryness under reduced pressure (1.0 kPa) at a temperature in the region of 30° C. The residue is taken up in 10 mL of diisopropyl ether, triturated and then reconcentrated to dryness. The solid obtained is dried in an oven under vacuum (0.01 kPa) at a temperature in the region of 60° C. 40 mg of N-[5-(N′-methyl-N′-phenylhydrazinocarbonyl)-1H-thieno[2,3-c]pyrazol-3-yl]-4-morpholin-4-ylmethylbenzamide are thus obtained in the form of an off-white solid melting at 242° C. MS-EI: 490(+)=M(+).

Provenance & Evidence