반응 #689603

ord-1b831301e89c48e1af27f7b167c5602c

반응 조건

온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The crude product was purified by chromatography on silica gel (Gradient elution: 100% CH2Cl2 to 93% CH2Cl2/7% MeOH)

실험 절차

A mixture of 1-(4-aminomethyl-pyridin-2-yl)-3-methyl-urea (3.8 g, 21.1 mmol) and 2-chloro-nicotinic acid methyl ester [Mann et al. J. Chem. Soc.; 1952; 2057, 2060] (1.78 g, 10.4 mmol) was heated for 1 hour at 120° C. The crude product was purified by chromatography on silica gel (Gradient elution: 100% CH2Cl2 to 93% CH2Cl2/7% MeOH) to give 2-{[2-(3-methyl-ureido)-pyridin-4-ylmethyl]-amino}-nicotinic acid methyl ester (2.06 g); Mp. 145-146° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07906533B2uspto-grants-2011_03