反应 #1135851

反应方程式

3-Amino-5-bromo pyridine

pyridine

isobutyryl chloride

→

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

收率 71.0%

溶剂

DCM

DCM

反应条件

后处理

1. 1
   洗涤washed with water
2. 2
   萃取The organic extract
3. 3
   其他was dried
4. 4
   浓缩concentrated
5. 5
   其他purified by column chromatography

实验过程

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).

来源