반응 #67521

반응 방정식

5-cyano-3-methyl-pyridine-2-carboxylic acid tert-butyl ester

1,3-dimethoxybenzene

TFA

→

title compound

5-cyano-3-methyl-pyridine-2-carboxylic acid

용매

toluene

반응 조건

후처리

1. 1
   기타evaporated
2. 2
   기타evaporated (2×)
3. 3
   기타The product was crystallized from TBME/hexanes

실험 절차

To a solution of 8.50 g (38.9 mmol) 5-cyano-3-methyl-pyridine-2-carboxylic acid tert-butyl ester in 51 ml (389 mmol) 1,3-dimethoxybenzene were added 85 ml TFA and stirred for 6.5 h. The reaction mixture was diluted with toluene and evaporated. The residue was taken up in toluene and evaporated (2×). The product was crystallized from TBME/hexanes to give the title compound as a white powder. HPLC: RtH1=2.314 min; ESIMS [M+Na]+=163; 1H-NMR (360 MHz, CDCl3): δ 8.77 (s, 1H), 8.07 (s, 1H), 2.87 (s, 3H).

출처