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HRID1606540

反应详情

EQUATION

反应方程式

HRID 1606540 的结构方程式

REACTANTS

反应物

3
结构：CCO
HCID702

Ethanol

C2H6O

结构：[Na+].[Na+].[S-2]
HCID14804

Disodium sulfide

Na2S

结构：CCOC(=O)c1c(C)nc(Cl)c([N+](=O)[O-])c1NCCCN(C)C
HCID53717160

未命名化合物

PRODUCTS

生成物

1
结构：CCOC(=O)c1c(C)nc(S)c([N+](=O)[O-])c1NCCCN(C)C
HCID178469259

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O
溶剂HCID962

Water

H2O

PROCEDURE

实验过程

34.5 g. of 4-[[3-(dimethylamino)propyl]amino]-6-chloro-2-methyl-5-nitropyridine-3-carboxylic acid, ethyl ester are dissolved in 100 ml. of ethanol. 15 g. of sodium sulfide in 10 ml. of water are added and the mixture is stirred without cooling for 1 hour. After this time, the precipitated 4-[[3-(dimethylamino)propyl]amino]-6-mercapto-2-methyl-5-nitropyridine-3-carboxylic acid, ethyl ester is filtered off and recrystallized from methanol, yield 18 g. (53%), m.p. 131°-132°.

WORKUP

后处理

  1. temperaturewithout cooling for 1 hour
  2. filtrationAfter this time, the precipitated 4-[[3-(dimethylamino)propyl]amino]-6-mercapto-2-methyl-5-nitropyridine-3-carboxylic acid, ethyl ester is filtered off
  3. customrecrystallized from methanol, yield 18 g