反应 #75562

ord-4a87912f4f5b4b53b7be1e8d5a52c856

反应方程式

O=C(O)c1ccccc1S
thiosalicylic acid
NCCN
ethylenediamine
CO
methanol
Sc1ccccc1C1=NCCN1
pure product
收率 53.1%
Sc1ccccc1C1=NCCN1
2-(4,5-Dihydro-1H-imidazol-2-yl)-benzenethiol
收率 53.1%

反应条件

温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was refluxed under nitrogen for 4 h
  2. 2
    workup.WAITto stand at 22° C. over night
  3. 3
    其他the resulting yellow crystalline solid collected
  4. 4
    洗涤washed with ether

实验过程

To a suspension of 20.0 g (0.112 mol) of thiosalicylic acid in 200 mL of 1,2-dichlorobenzene was added 21.6 mL (0.323 mol) of ethylenediamine. The mixture was refluxed under nitrogen for 4 h then cooled to ca. 60° C. and 50 mL of methanol was added. The solution was allowed to stand at 22° C. over night and the resulting yellow crystalline solid collected and washed with ether to give 10.6 g of pure product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06699873B1uspto-grants-2004_03