반응 #6977

반응 방정식

sodium ethoxide

ethyl-6-amino-nicotinate

benzoyl isothiocyanate

→

6-thioureido-nicotinic acid ethyl ester

수율 77.0%

용매

ethanol

THF

반응 조건

후처리

1. 1
   기타the volatiles were removed in vacuo
2. 2
   기타the solid formed
3. 3
   여과was collected by filtration
4. 4
   세척rinsed with water
5. 5
   기타dried

실험 절차

A mixture of ethyl-6-amino-nicotinate (2.5 g, 15 mmol) and benzoyl isothiocyanate (2.45 g, 15 mmol) in THF (20 mL) was heated at 40° C. for 4 h. To this mixture at RT, was added sodium ethoxide (2.04 g, 30 mmol) in ethanol (10 mL). After stirring the resulting mixture at RT for 16 h, the volatiles were removed in vacuo. The residue was suspended in aqueous NH4Cl and the solid formed was collected by filtration, rinsed with water and dried to afford 6-thioureido-nicotinic acid ethyl ester as a white solid (2.6 g, 77% yield). LC/MS; (M+H)+=226.

출처