반응 #77549

반응 방정식

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

용매

THF

THF

반응 조건

후처리

1. 1
   기타The product was precipitated from ether
2. 2
   기타to form the white solid
3. 3
   기타The solid thus obtained
4. 4
   세척was washed sequentially with ether, methanol and acetone

실험 절차

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%).

출처