HRID1658524

反应详情

EQUATION

反应方程式

HRID 1658524 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6.2 g. of 4-sec.butylamino-6-mercapto-2-methyl-5-nitropyridine-3-carboxylic acid, ethyl ester are dissolved in 50 ml. of acetic acid. Iron dust is added carefully at reflux temperature until the mixture is colorless. The excess of iron is filtered off and the filtrate is evaporated to dryness. The oily residue is dissolved in 10 ml. of methanol and precipitated by the addition of aqueous ammonia to obtain 5-amino-4-sec.butylamino-6-mercapto-2-methylpyridine-3-carboxylic acid, ethyl ester, yield 3 g. (53%); m.p. 88°-89° (ethyl acetate).

WORKUP

后处理

  1. temperatureat reflux temperature until the mixture
  2. filtrationThe excess of iron is filtered off
  3. customthe filtrate is evaporated to dryness
  4. dissolutionThe oily residue is dissolved in 10 ml
  5. customof methanol and precipitated by the addition of aqueous ammonia