HRID1295586

反应详情

EQUATION

反应方程式

HRID 1295586 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was prepared by reaction of 4-methanesulfonyl-6-(piperazin-1-ylmethyl)-3,4-dihydro-2H-benzo[1,4]oxazine (0.145 g, 1 mmol), 5-(2-bromoethoxy)-2-methylquinoline (0.266 g, 1 mmol) and N,N-diisopropylethylamine (1.29 g, 10 mmol) in isopropyl alcohol (8 mL). The mixture was heated at reflux with stirring in a reaction block for 48 h. The reaction mixture was cooled, and the isopropyl alcohol evaporated in vacuo. The residue was partitioned between dichloromethane (5 mL), and water (5 mL). The organic layer was added onto a 10 g pre-packed silica column and eluted with 0–10% methanol in ethyl acetate. Fractions containing desired material were combined and evaporated in vacuo to give the title compound (0.180 g, 36%) as a colourless solid. Mass Spectrum (APCl+): Found 497 (MH+). C28H32N4O4S requires 496.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux
  3. temperatureThe reaction mixture was cooled
  4. customthe isopropyl alcohol evaporated in vacuo
  5. customThe residue was partitioned between dichloromethane (5 mL), and water (5 mL)
  6. additionThe organic layer was added onto a 10 g pre-packed silica column
  7. washeluted with 0–10% methanol in ethyl acetate
  8. additionFractions containing desired material
  9. customevaporated in vacuo