反应 #805489

ord-3ed48da16305459d89a46facae4ad78d

溶剂

反应条件

温度
125°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling down to room temperature
  2. 2
    过滤The solid was filtered off
  3. 3
    洗涤washed with water
  4. 4
    其他dried
  5. 5
    其他The crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 10:1)

实验过程

A mixture of ethyl 2-aminothiophene-3-carboxylate (0.5 g, 3.18 mmol), chloroformamidine hydrochloride (0.91 g, 7.95 mmol) and dimethylsulfone (1.50 g, 15.9 mmol) was heated at 120-130° C. for 30 minutes. After cooling down to room temperature, water (10 ml) was added and ammonium hydroxide was used to neutralize the suspension. The solid was filtered off, washed with water and dried. The crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 10:1) to yield the title compound as a white solid (0.24 g, 45%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09193741B2uspto-grants-2015_11