تفاعل #71402

معادلة التفاعل

5-bromo-8-(2-fluoro-3,5-dimethoxy-phenyl)-quinoxaline

CuCN

→

title compound

المردود 62.0%

8-(2-Fluoro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonitrile

المردود 62.0%

المذيبات

DCM

NMP

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto cool to rt
2. 2
   ترشيحfiltered through celite
3. 3
   استخلاصthe filtrate extracted with DCM
4. 4
   غسيلThe organic phase was washed with H2O and brine
5. 5
   تجفيفdried (Na2SO4)
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated
8. 8
   أخرىThe residue was triturated in DCM

الإجراء التجريبي

A mixture of 5-bromo-8-(2-fluoro-3,5-dimethoxy-phenyl)-quinoxaline (Step 94.3) (3.09 g, 8.5 mmol) and CuCN (918 mg, 10.2 mmol, 1.2 equiv) in NMP (30 mL) was stirred for 6.5 h at 160° C., under an argon atmosphere. The reaction mixture was allowed to cool to rt, diluted with DCM/(10% aqueous solution of ethylenediamine) (200 mL, v/v 1:1), filtered through celite and the filtrate extracted with DCM. The organic phase was washed with H2O and brine, dried (Na2SO4), filtered and concentrated. The residue was triturated in DCM to provide 1.63 g of the title compound as a white solid: ESI-MS: 310.1 [M+H]+; tR=4.41 min (System 1).

المصدر