反应 #2320165

ord-c5763d20d98f444aa94d1608dce5d7fb

反应方程式

O=C(O)C(F)(F)F
Trifluoroacetic acid
CC(C)(C)OC(=O)N1CCCN(c2ncccc2CNc2nncn2-c2cccc(Cl)c2Cl)CC1
solution
CC(C)(C)OC(=O)N1CCCN(c2ncccc2CNc2nncn2-c2cccc(Cl)c2Cl)CC1
4-(3-{[4-(2,3-Dichloro-phenyl)-4H-[1,2,4]triazol-3-ylamino]-methyl}-pyridin-2-yl)[1,4]diazepane-1-carboxylic acid tert-butyl ester
Clc1cccc(-n2cnnc2NCc2cccnc2N2CCCNCC2)c1Cl
title compound
Clc1cccc(-n2cnnc2NCc2cccnc2N2CCCNCC2)c1Cl
N-{[2-(1,4-diazepan-1-yl)pyridin-3-yl]methyl}-4-(2,3-dichlorophenyl)-4H-1,2,4-triazol-3-amine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the ice bath was removed
  2. 2
    workup.ADDITIONThe reaction mixture was diluted with dichloromethane
  3. 3
    洗涤The organic was washed with saturated sodium bicarbonate
  4. 4
    其他The layers were separated
  5. 5
    萃取the aqueous layer was extracted with dichloromathane
  6. 6
    洗涤The combined organic layer was washed with brine
  7. 7
    干燥dried over magnium sulfate
  8. 8
    过滤filtered
  9. 9
    浓缩concentrated

实验过程

Trifluoroacetic acid (15 mL) was added to a solution of Example 112C (2.0 g, 3.86 mmol) in dichloromethane (75 mL) at 0° C. 5 minuted later, the ice bath was removed and the reaction mixture was stirred at room temperature for 16 hours. The reaction mixture was diluted with dichloromethane. The organic was washed with saturated sodium bicarbonate and the pH was adjusted to 9. The layers were separated and the aqueous layer was extracted with dichloromathane. The combined organic layer was washed with brine, dried over magnium sulfate, filtered and concentrated to yield the title compound that was used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07709469B2uspto-grants-2010_05