反应 #84069

ord-3b909b9459f547ddaf88c07c65870078

反应方程式

N#Cc1ccc(-c2ccc3cc(O)ccc3n2)cc1
4-(6-hydroxyquinolin-2-yl)benzonitrile
Cl.NO
NH2OH.HCl
N=C(NO)c1ccc(-c2ccc3cc(O)ccc3n2)cc1
desired product
收率 78.0%
N=C(NO)c1ccc(-c2ccc3cc(O)ccc3n2)cc1
N-hydroxy-4-(6-hydroxyquinolin-2-yl)benzimidamide
收率 78.0%

溶剂

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩followed by concentration in vacuo
  2. 2
    workup.STIRRINGstirred for 1 hour
  3. 3
    过滤Filtration
  4. 4
    其他drying of the solids

实验过程

See Scheme 4, route B. 4-(6-hydroxyquinolin-2-yl)benzonitrile (900 mg, 3.68 mmol) was dissolved in 25 mL of EtOH and to it was added NH2OH.HCl (500 mg, 7.36 mmol) and TEA (1.5 mL). The mixture was stirred at 80° C. for 2 hours followed by concentration in vacuo. The crude solids were then suspended in 25 mL of H2O and stirred for 1 hour. Filtration and drying of the solids yielded desired product (800 mg, 78% yield).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09433618B2uspto-grants-2016_09