HRID1406291

反应详情

EQUATION

反应方程式

HRID 1406291 的结构方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1-Chloropropan-2-one (0.334 mL, 4.20 mmol) and methyl 2-amino-2-thioxoacetate (500 mg, 4.20 mmol) was dissolved in EtOH. The reaction solution was heated to 80° C. for overnight, cooled to RT, concentrated and purified with a silica gel column by ISCO CombiFlash® chromatography eluting with 10%-35% EtOAc/Haptane to give the title compound as a yellowish oil (243 mg, 33.8%) as the ethyl ester. A methyl ester product was isolated as a yellow solid (104 mg, 15.8%).

WORKUP

后处理

  1. temperaturecooled to RT
  2. concentrationconcentrated
  3. custompurified with a silica gel column by ISCO CombiFlash® chromatography
  4. washeluting with 10%-35% EtOAc/Haptane