反応 #71332

反応方程式

4-(4-{[8-(2,6-dichloro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonyl]-amino}-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

HCl

→

title compound

収率 80.2%

8-(2,6-Dichloro-3,5-dimethoxy-phenyl)-quinoxaline-5-carboxylic acid (4-piperazin-1-yl-phenyl)-amide

収率 80.2%

溶媒

DCM

H2O

dioxane

反応条件

後処理

1. 1
   その他The aqueous layer was separated
2. 2
   抽出extracted with DCM
3. 3
   洗浄The organic phase was washed with H2O and brine
4. 4
   乾燥dried (Na2SO4)
5. 5
   ろ過filtered
6. 6
   濃縮concentrated
7. 7
   その他The residue was triturated in Et2O

実験手順

A mixture of 4-(4-{[8-(2,6-dichloro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonyl]-amino}-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (Step 8.1) (137 mg, 0.22 mmol) and a 4 N solution of HCl in dioxane (5 mL) was stirred for 1 h at rt. The reaction mixture was diluted with DCM and H2O. The aqueous layer was separated and extracted with DCM. The organic phase was washed with H2O and brine, dried (Na2SO4), filtered and concentrated. The residue was triturated in Et2O to afford 95 mg of the title compound as a red solid: ESI-MS: 537.9/539.9 [M+H]+; tR=4.01 min (System 1).

出典