反应 #77549

反应方程式

N-(2-phenyl-2-hydroxyethyl)-N′-cyano-N″-4-pyridylguanidine

triphenylphosphine

diisopropyl azodicarboxylate

→

Compound 14

[5-phenyl-1-(4-pyridyl)tetrahydro-1H-2-imidazolyliden]aminomethane-nitrile

溶剂

THF

THF

反应条件

后处理

1. 1
   其他The product was precipitated from ether
2. 2
   其他to form the white solid
3. 3
   其他The solid thus obtained
4. 4
   洗涤was washed sequentially with ether, methanol and acetone

实验过程

To a solution of N-(2-phenyl-2-hydroxyethyl)-N′-cyano-N″-4-pyridylguanidine (1.0 g, 3.56 mmol) and triphenylphosphine (1.86 g, 7.12 mmol) in THF (30 mL) at 0° C. was added diisopropyl azodicarboxylate (3.8 mL, 7.12 mmol) dissolved in 15 mL (THF) by syringe pump over 30 min. The resulting mixture was kept stirring and warmed to room temperature for 70 h. The product was precipitated from ether to form the white solid. The solid thus obtained was washed sequentially with ether, methanol and acetone to give the product (i.e., Compound 14) as a white solid (0.67 g, 72%).

来源