HRID1925185

反应详情

EQUATION

反应方程式

HRID 1925185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 1-amino-naphthalene-2-thiol in pyridine are added two mol equivalents of 1-methyl-cyclohexanecarbonyl chloride at room temperature. After completion of the addition, the reaction mixture is heated to 60° C. for 2 hours. The pyridine is then removed under reduced pressure, water is added and the mixture is extracted with ethyl acetate. The combined extracts are washed with sat. NaHCO3-solution, diluted hydrochloric acid and brine, dried (Na2SO4) and concentrated to obtain crude 1-methyl-cyclohexanecarbothioic acid S-{1-[(1-methyl-cyclohexanecarbonyl)-amino]-naphthalen-2-yl}ester.

WORKUP

后处理

  1. additionAfter completion of the addition
  2. customThe pyridine is then removed under reduced pressure, water
  3. additionis added
  4. extractionthe mixture is extracted with ethyl acetate
  5. washThe combined extracts are washed with sat. NaHCO3-solution, diluted hydrochloric acid and brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated