HRID2058857

反应详情

EQUATION

反应方程式

HRID 2058857 反应方程式

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

Ethyl N-(5-propyl-7-cyano-4,5,6,7-tetrahydrobenzothiazol-2-yl)carbamate (0.08 mol) and the dimethyl acetal of 2-but-3-enylaminoacetaldehyde (30 ml.) as charged into a glass reaction vessel equipped with a stirrer, reflux condenser and gas addition tube. The reaction mixture is blanketed with nitrogen gas and is heated 125° C. for a period of about 8 hours. After this time the reaction mixture is distilled to remove excess starting material. The residue is purified by elution chromatography using ethyl acetate as the eluant. The chromatographed solution is then stripped of solvent to yield the desired product dimethyl acetal of 2-[1-but-3-enyl-3-(5-propyl-7-cyano-4,5,6,7-tetrahydrobenzothiazol-2-yl)ureido]acetaldehyde.

WORKUP

后处理

  1. customequipped with a stirrer
  2. temperaturereflux
  3. additioncondenser and gas addition tube
  4. distillationAfter this time the reaction mixture is distilled
  5. customto remove excess
  6. customThe residue is purified by elution chromatography