HRID867967

反应详情

EQUATION

反应方程式

HRID 867967 的结构方程式

PROCEDURE

实验过程

Then, 2.0 g of the resulting anilinium 2-mercaptobenzenesulfonate was subjected to ion-exchange column chromatography (about 30 ml of Dowex 50W-X2, 100-200 mesh, H-form was filled into a column) and eluted with a mixed solvent of methanol and water (4/1, v/v). Acidic fractions were concentrated under reduced pressure, and about 50 ml of isopropanol was added to the resulting syrup. The solvent was evaporated under reduced pressure. To 1.1 g of the resulting syrup, about 4 ml of isopropanol was added to form a solution. Triethylamine (0.58 g) was added to the solution, and the resulting crystals were collected by filtration to give 0.84 g of the captioned compound as colorless crystals (melting point: 89° to 90° C.)

WORKUP

后处理

  1. additionwas filled into a column) and
  2. washeluted with a mixed solvent of methanol and water (4/1
  3. concentrationAcidic fractions were concentrated under reduced pressure, and about 50 ml of isopropanol
  4. additionwas added to the resulting syrup
  5. customThe solvent was evaporated under reduced pressure
  6. additionTo 1.1 g of the resulting syrup, about 4 ml of isopropanol was added
  7. customto form a solution
  8. filtrationthe resulting crystals were collected by filtration