Реакция #533372

ord-3ff0b12fbafb49e3933e4f1323277a52

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеAfter partition
  2. 2
    Экстракцияthe aqueous phase was extracted with 20 mL of dichloromethane
  3. 3
    Промывкаwashed with water twice
  4. 4
    Сушкаdried over sodium sulfate
  5. 5
    ДругоеThe solvent was removed
  6. 6
    Другоеthe residue was purified by flash chromatography

Методика

To a solution of 2-cyano-6-(3-bromomethylbenzyloxy)benzothiazole (1 g, 2.8 mmol) in 20 mL of dichloromethane was added 1-phenylpiperazine (1.7 mL, 11.2 mmol) dropwise. The resultant solution was stirred at RT for 30 minutes. Then, 20 mL of saturated sodium bicarbonate solution was added. After partition, the aqueous phase was extracted with 20 mL of dichloromethane. The organic extracts were combined, washed with water twice and dried over sodium sulfate. The solvent was removed and the residue was purified by flash chromatography using 1% methanol in dichloromethane. 594 mg of product was obtained.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08476450B2uspto-grants-2013_07