反应 #66094

ord-0de23b60befe437f8b5091e03c28af87

反应方程式

CCN=C=NCCCN(C)C.Cl
1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride
CN(C)c1ccccn1
dimethylaminopyridine
CC#N
acetonitrile
C1CCCCC(N2CCCCCCCN2)CCC1
diazabicyclononane
O
water
O=C(c1c[nH]c2nc(Cl)ccc12)N1CCN2CCC1CC2
crystalline compound
O=C(c1c[nH]c2nc(Cl)ccc12)N1CCN2CCC1CC2
6-Chloro-3-(1,4-diazabicyclo[3.2.2]non-4-ylcarbonyl)-1H-pyrrolo[2,3-b]pyridine

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with dichloromethane
  2. 2
    其他the organic phase is evaporated

实验过程

375 mg (2 mmol) of the derivative from the preceding step, 760 mg (4 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, 50 mg of dimethylaminopyridine, 5 ml of acetonitrile and 500 mg (4 mmol) of diazabicyclononane are placed in a microwave tube (Personal Chemistry), and the tube is stoppered and heated at 100° C. for 10 minutes. The mixture is immersed in 50 ml of water and extracted with dichloromethane, and the organic phase is evaporated. By trituration in isopropyl ether, 310 mg of a crystalline compound are obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08524706B2uspto-grants-2013_09