HRID579456

反应详情

EQUATION

反应方程式

HRID 579456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2-Bromo-6-hydroxybenzothiazole (345 mg, 1.5 mmol), 1-isopropyl-piperazine hydrochloride (271 mg, 1.65 mmol) and dry potassium carbonate (828 mg, 6.00 mmol), were dissolved in 6 mL, of dry N,N-dimethylformamide. The resulted pale brown solution was stirred at 100° C. for 18 h in a closed vial. The reaction mixture was evaporated, suspended in 20 mL of water and extracted with dichloromethane (3×15 mL). The combined organic layers were washed with saturated sodium bicarbonate and brine, then dried over MgSO4. After evaporation the residue was purified by column chromatography (Kieselgel 60) using chloroform-methanol 49:1 as the eluent. The title compound (76 mg, 0.27 mmol, 18%) was obtained as a white solid.

WORKUP

后处理

  1. customThe reaction mixture was evaporated
  2. extractionextracted with dichloromethane (3×15 mL)
  3. washThe combined organic layers were washed with saturated sodium bicarbonate and brine
  4. dry with materialdried over MgSO4
  5. customAfter evaporation the residue
  6. customwas purified by column chromatography (Kieselgel 60)