HRID1030

反应详情

EQUATION

反应方程式

HRID 1030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

H2S gas is passed, at -10°, into a solution of 1.2 g of 3-p-cyanophenyl-5-(p-methoxycarbonyimethylphenoxymethyl)oxazolidin-2-one (obtainable in accordance with Example 1) in 50 ml of pyridine and 7 ml of triethylamine. The mixture is subsequently stirred at room temperature for 14 h and concentrated by evaporation; the residue is dissolved in 50 ml of acetone and treated with 9 ml of methyl iodide. After this mixture has been stirred for a further 6 h, it is filtered and the residue is washed with 5 ml of acetone and dissolved in 30 ml of methanol; 4.6 g of ammonium acetate are added to this solution, which is stirred at room temperature for 24 h. Following the customary working-up, 3-p-amidinophenyl-5-(p-methoxycarbonylmethylphenoxymethyl)oxazolidin-2-one (semihydriodide) is obtained, M.p. 151°-152°.

WORKUP

后处理

  1. concentrationconcentrated by evaporation
  2. dissolutionthe residue is dissolved in 50 ml of acetone
  3. additiontreated with 9 ml of methyl iodide
  4. stirringAfter this mixture has been stirred for a further 6 h
  5. filtrationit is filtered
  6. washthe residue is washed with 5 ml of acetone
  7. dissolutiondissolved in 30 ml of methanol
  8. addition4.6 g of ammonium acetate are added to this solution, which
  9. stirringis stirred at room temperature for 24 h