반응 #156108

반응 방정식

3-Amino-5-bromo pyridine

pyridine

isobutyryl chloride

→

N-(5-bromopyridin-3-yl)isobutyramide

수율 71.0%

용매

DCM

DCM

반응 조건

후처리

1. 1
   세척washed with water
2. 2
   추출The organic extract
3. 3
   기타was dried
4. 4
   농축concentrated
5. 5
   기타purified by column chromatography

실험 절차

3-Amino-5-bromo pyridine (XVIII) (1 eq) was dissolved in DCM and cooled to 0° C. before adding pyridine (2.2 eq) and isobutyryl chloride (XIX) (1.1 eq). The reaction mixture was stirred at r.t. for 15 h until TLC showed the reaction was complete. The reaction mixture was diluted with DCM and washed with water. The organic extract was dried, concentrated and purified by column chromatography using silica gel (100-200 mesh) to afford N-(5-bromopyridin-3-yl)isobutyramide (XX) as a off white solid, (71% yield). 1H NMR (CDCl3) δ ppm 8.55-8.35 (m, 3H), 7.32 (s, 1H), 2.59-2.48 (m, 1H), 1.28-1.27 (d, 6H); ESIMS found C9H11BrN2O m/z 243.05 (M+H).

출처