HRID656640

反应详情

EQUATION

反应方程式

HRID 656640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

To a slurry of 3-amino-5-chloro-4-methyl-6-methylsulfanyl-thieno[2,3-b]pyridine-2-carboxylic acid cyclopropylamide (7.5 g, 22.87 mmol) in glacial acetic acid (75 ml) is added a solution of 30% hydrogen peroxide in water (2.85 ml, 25.16 mmol). The mixture is stirred at 35° C. for 16 hour, cooled to room temperature, and poured over water (300 ml). A bright yellow precipitate is formed. The mixture is stirred at 0° C. for 1 hour then the solid is collected by filtration and dried under vacuum at 60° C. for 3 hours to afford the title compound as a bright yellow solid (5.58 g, 71%). Mass (m/z): 344.1 (M++1).

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. customA bright yellow precipitate is formed
  3. stirringThe mixture is stirred at 0° C. for 1 hour
  4. filtrationthe solid is collected by filtration
  5. customdried under vacuum at 60° C. for 3 hours