HRID616513

反应详情

EQUATION

反应方程式

HRID 616513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture containing 60 g of 3-amino-2-cyano-3-(ethylmethylamino)propenethioamide and 250 ml of ethanol was heated to reflux, while 40 ml of 30% hydrogen peroxide (11.1 g of active H2O2) were added dropwise at such a rate as to maintain an even reflux. After the peroxide addition was completed, the reaction mixture was heated for 30 minutes. Charcoal was added to the hot solution. The charcoal was removed by filtration and the filtrate was evaporated under reduced pressure. The residue was recrystallized from toluene to yield 51 g of 5-amino-4-cyano-3-(ethylmethylamino)isothiazole, mp 94°-95°. The ir and nmr spectra were consistent with the assigned structure.

WORKUP

后处理

  1. temperaturewas heated
  2. additionwere added dropwise at such a rate as
  3. temperatureto maintain
  4. temperaturean even reflux
  5. temperaturethe reaction mixture was heated for 30 minutes
  6. customThe charcoal was removed by filtration
  7. customthe filtrate was evaporated under reduced pressure
  8. customThe residue was recrystallized from toluene