huagongshe.com
HRID1927575

反应详情

EQUATION

反应方程式

HRID 1927575 的结构方程式

REACTANTS

反应物

3
结构：O=C([O-])[O-].[K+].[K+]
HCID11430

Potassium Carbonate

CK2O3

结构：CCOc1c(OCC)c(=O)c1=O
HCID123228

Squaric acid diethyl ester

C8H10O4

结构：CN(C)C(=O)c1cccc(N)c1O
HCID16098483

3-Amino-2-hydroxy-N,N-dimethylbenzamide

C9H12N2O2

PRODUCTS

生成物

1
结构：CCOc1c(Nc2cccc(C(=O)N(C)C)c2O)c(=O)c1=O
HCID11855414

3-[(2-Ethoxy-3,4-dioxocyclobut-1-en-1-yl)amino]-2-hydroxy-N,N-dimethylbenzamide

C15H16N2O5

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CCO
溶剂HCID702

Ethanol

C2H6O

结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

44 g of 3-amino-2-hydroxy-N,N-dimethyl-benzamide are dissolved in 880 ml of EtOH. 46 g of 3,4-diethoxy-3-cyclobuten-1,2-dione and 4.4 g of K2CO3 are added and the reaction mixture obtained is stirred overnight at rt. Solvent is evaporated. A residue obtained is purified by column chromatography over 500 g of silica using CH2Cl2/MeOH 98/2 as eluent. The product-containing fractions are combined and solvent is evaporated. A residue obtained is suspended in 1 l of MeOH and filtered. This process is repeated a further 3 times. The title compound is obtained.

WORKUP

后处理

  1. customthe reaction mixture obtained
  2. customSolvent is evaporated
  3. customA residue obtained
  4. customis purified by column chromatography over 500 g of silica
  5. customsolvent is evaporated
  6. customA residue obtained
  7. filtrationfiltered