反应 #1129733

ord-bd085724012041e6b953d5889ae4e57d

反应条件

温度
40°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture is heated at the boil for 68 hours
  2. 2
    温度After cooling
  3. 3
    其他The precipitate formed
  4. 4
    过滤is filtered off with suction
  5. 5
    洗涤washed with water
  6. 6
    其他dried in vacuo

实验过程

1.2 104 mg (0.75 mmol) of potassium carbonate are added to a solution of 103 mg (0.30 mmol of tert-butyl 3-(3-trimethylsilylpropynoyl)pyrrolo-[3,2-c]pyridine-1-carboxylate and 148 mg (0.75 mmol) of phenylguanidine carbonate in 1.5 ml of ethylene glycol monomethyl ether, and the mixture is heated at the boil for 68 hours. After cooling, 10 ml of water are added, and the mixture is stirred at 40° C. for 1 h. The precipitate formed is filtered off with suction, washed with water and dried in vacuo, giving phenyl-[4-(1H-pyrrolo[3,2-c]pyridin-3-yl)pyrimidin-2-yl]amine (“A1”) as pale-brown solid; ESI 287;

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08557977B2uspto-grants-2013_10