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HRID270694

反应详情

EQUATION

反应方程式

HRID 270694 的结构方程式

REACTANTS

反应物

2
结构：O=C([O-])[O-].[Na+].[Na+]
HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

结构：O=Cc1cnccc1NC(=O)Cc1c(Cl)ccc([N+](=O)[O-])c1Cl
HCID59833859

未命名化合物

PRODUCTS

生成物

1
结构：O=c1[nH]c2ccncc2cc1-c1c(Cl)ccc([N+](=O)[O-])c1Cl
HCID59833918

未命名化合物

收率 79%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

A solution of 2-(2,6-dichloro-3-nitro-phenyl)-N-(3-formyl-pyridin-4-yl)-acetamide (5.0 g, 14.12 mmol) and Na2CO3 (2.5 g) in MeOH (300 mL) is heated for 15 minutes at 70° C. After filtration of the reaction mixture, the solvent is removed by concentration to give crude product, which is purified by flash silica gel column elute with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (93/7%) to give the titled intermediate as a solid (3.75 g, 77.7%).

WORKUP

后处理

  1. filtrationAfter filtration of the reaction mixture
  2. customthe solvent is removed by concentration
  3. customto give crude product, which
  4. customis purified by flash silica gel column
  5. washelute with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (93/7%)