HRID704633

反应详情

EQUATION

反应方程式

HRID 704633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 6-(1-piperazinyl)-3,4-dihydro-2(1H)-quinolinone (1.28 g), 4-chloro-6,7-dimethoxyquinazoline hydrochloride (1.43 g) and N,N-dimethylformamide (50 ml) was added triethylamine (560 mg) and the mixture was stirred for 8 hours at ambient temperature. The solvent was removed under reduced pressure and to the obtained residue were added water (20 ml), tetrahydrofuran (10 ml) and ethyl acetate (10 ml). The separated organic layer was washed with brine, dried over magnesium sulfate and concentrated. The residue was subjected to a column chromatography on silica gel (80 g) and eluted with 10% solution of methanol in chloroform. The fractions containing the object compound were combined and concentrated. The obtained residue was subjected to a column chromatography on alumina (60 g) and eluted with 5% solution of methanol in chloroform. The fractions containing the object compound were combined and concentrated to give 6-[4-(6,7-dimethoxyquinazolin-4-yl)-1-piperazinyl]-3,4-dihydro-2(1H)-quinolinone (0.8 g).

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure and to the obtained residue
  2. additionwere added water (20 ml), tetrahydrofuran (10 ml) and ethyl acetate (10 ml)
  3. washThe separated organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. washeluted with 10% solution of methanol in chloroform
  7. additionThe fractions containing the object compound
  8. concentrationconcentrated
  9. washeluted with 5% solution of methanol in chloroform
  10. additionThe fractions containing the object compound
  11. concentrationconcentrated