HRID1437748

反应详情

EQUATION

反应方程式

HRID 1437748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 2′,6′-dichloro-3,4,5,6-tetrahydro-2H-[1,4′]bipyridinyl (500 mg, 2.15 mmol) in toluene (6 mL) were added potassium tert-butoxide (486 mg, 4.3 mmol), palladium(II) acetate (24 mg, 0.1 mmol), BINAP (67 mg, 0.1 mmol), and 4-amino-N-methylbenzenesulfonamide (444 mg, 2.15 mmol) were taken in a 10 mL reaction vessel. This reaction mixture was subjected the microwave irradiation, in which the microwave power was 250 W, to attain a reaction temperature of 1 50° C. After this reaction proceeded for 30 min, water (200 mL) was added to the reaction mixture and the reaction product was extracted with ethyl acetate. The organic layer was dried over sodium sulphate, filtered, and the filtrate concentrated under vacuum. The product was purified through column chromatography using 230-400 mesh silica gel to afford the desired compound as light yellow solid (290 mg, yield, 35%).

WORKUP

后处理

  1. customwere taken in a 10 mL reaction vessel
  2. customthe microwave irradiation
  3. customa reaction temperature of 1 50° C
  4. extractionthe reaction product was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over sodium sulphate
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated under vacuum
  8. customThe product was purified through column chromatography