반응 #365756

반응 방정식

6-tert-butoxycarbonylaminothionicotinamide

ethyl 2-chloro-acetoacetate

sodium acetate

sodium hydrogen carbonate

→

ethyl 2-(6-tert-butoxycarbonylamino-3-pyridyl)-4-methyl-5-thiazolecarboxylate

수율 27.6%

용매

ethanol

water

반응 조건

후처리

1. 1
   온도was heated for 2 hours
2. 2
   온도under reflux
3. 3
   여과The precipitated crystals were collected by filtration
4. 4
   세척the crystals were successively washed with water, ethanol and ether

실험 절차

A mixture of 6-tert-butoxycarbonylaminothionicotinamide (506 mg), ethyl 2-chloro-acetoacetate (492 mg) and sodium acetate (252 mg) in ethanol (20 ml) was heated for 2 hours under reflux, and to the mixture were added sodium hydrogen carbonate aqueous solution and water. The precipitated crystals were collected by filtration, and the crystals were successively washed with water, ethanol and ether to give ethyl 2-(6-tert-butoxycarbonylamino-3-pyridyl)-4-methyl-5-thiazolecarboxylate (200 mg).

출처