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HRID1774949

反应详情

EQUATION

反应方程式

HRID 1774949 的结构方程式

REACTANTS

反应物

3
结构：O=C([O-])[O-].[Na+].[Na+]
HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

结构：Cc1cc(Br)ncc1[N+](=O)[O-]
HCID345873

2-Bromo-4-methyl-5-nitropyridine

C6H5BrN2O2

结构：OB(O)c1cccnc1
HCID2734378

3-Pyridinylboronic acid

C5H6BNO2

PRODUCTS

生成物

1
结构：Cc1cc(-c2cccnc2)ncc1[N+](=O)[O-]
HCID46316008

未命名化合物

收率 80%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：Cl[Pd]Cl.[Fe+2].c1ccc(P(c2ccccc2)[c-]2cccc2)cc1.c1ccc(P(c2ccccc2)[c-]2cccc2)cc1
催化剂HCID178418228

Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)

C34H28Cl2FeP2Pd

结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

PROCEDURE

实验过程

To a solution of 2-bromo-4-methyl-5-nitropyridine (217 g, 1 mol) in DMF (2000 mL) was added Pd(dppf)Cl2 (5 g), saturated solution of Na2CO3 (200 mL) and pyridin-3-ylboronic acid (147 g, 1.2 mol). The mixture was stirred under argon for 6 h at 100. After cooling down, the solvent was removed under reduced pressure evaporation and the residue was purified by silica-gel column chromatography (mobile phase: EA:PE=1:1) to afford 4-methyl-5-nitro-2,3′-bipyridine (172 g, 80%).

WORKUP

后处理

  1. temperatureAfter cooling down
  2. customthe solvent was removed under reduced pressure evaporation
  3. customthe residue was purified by silica-gel column chromatography (mobile phase: EA:PE=1:1)