反应 #2320118

ord-59c2543ddad944bba9ceca3f296f3eb5

反应方程式

ClCCl
CH2Cl2
CN(C)S(=O)(=O)c1cc(Br)c(F)cc1F
5-Bromo-2,4-difluoro-N,N-dimethyl-benzenesulfonamide
OB(O)c1ccncc1
4-pyridine-boronic acid
O=C([O-])[O-].[Na+].[Na+]
Na2CO3
CN(C)S(=O)(=O)c1cc(-c2ccncc2)c(F)cc1F
2,4-Difluoro-N,N-dimethyl-5-pyridin-4-yl-benzenesulfonamide

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤the organic phase was washed with water
  2. 2
    干燥dried (MgSO4)
  3. 3
    过滤filtered
  4. 4
    其他evaporated to dryness
  5. 5
    其他The residue was then used without any further purification

实验过程

5-Bromo-2,4-difluoro-N,N-dimethyl-benzenesulfonamide (400 mg) and 4-pyridine-boronic acid (165 mg) was dissolved in toluene (5 ml) and abs EtoH (5 ml). To the mixture was then added Na2CO3 (200 mg) and Pd(PPh3)4 (79 mg) under an atmosphere of Argon. The resulting mixture was heated to 90° C. for 18 h. Then CH2Cl2 was added and the organic phase was washed with water and dried (MgSO4), filtered and evaporated to dryness. The residue was then used without any further purification. (MS m/z (rel. intensity, 70 eV) 298 (M+, 77), 256 (36), 191 (bp), 190 (98), 143 (74).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE041315E1uspto-grants-2010_05