HRID1111057

反应详情

EQUATION

反应方程式

HRID 1111057 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 36 g. of 1-ethylthiourea in 200 ml. of acetone was added 70 g. of methyliodide. Evaporation of the solvent gave 71 g. of 1-ethyl-2-methylisothiourea hydroiodide as colorless crystals, m.p. 84°-87° C. This isothiurea, 23.2 g., was reacted with a total of 30 ml. of benzoyl chloride and after 6 hours the solution was poured onto ice. The mixture was made basic with NaOH and the crystals which formed were collected by filtration to give 27.8 g. of 1,3-bisbenzoyl-1-ethyl-2-methylisothiourea, m.p. 84°-86° C. This bisbenzoylisothiourea, 3.1 g., was reacted with 2.4 g. of 4-aminomethylbenzenesulfonamide hydrochloride and 1.5 g. of sodium acetate in 250 ml. of isopropyl alcohol. Aqueous work-up followed by dichloromathane extraction and evaporation gave the title compound as a colorless glass, m.p. 70°-80° C.

WORKUP

后处理

  1. customEvaporation of the solvent
  2. customgave 71 g
  3. custom, was reacted with a total of 30 ml
  4. customthe crystals which formed
  5. filtrationwere collected by filtration
  6. customto give 27.8 g
  7. custom, was reacted with 2.4 g
  8. extractionAqueous work-up followed by dichloromathane extraction and evaporation