Реакция #41695

Уравнение реакции

2-mercaptoethanol

potassium carbonate

N,N-dimethylformamide

6-(1-acetylpyrrolidin-2-yl)-5-(6-chloropyridin-3-yl)oxy-2-pyridin-2-yl-1H-benzimidazole

6-(1-Acetylpyrrolidin-2-yl)-5-((6-chloropyridin-3-yl)oxy)-2-pyridin-2-yl-1H-benzimidazole

→

compound

2-(5-((6-(1-Acetylpyrrolidin-2-yl)-2-pyridin-2-yl-1H-benzimidazol-5-yl)oxy)pyridin-2-ylsulfanyl)ethanol

Растворители

sodium bicarbonate

Условия реакции

Обработка

1. 1
   Другоеthe reaction liquid
2. 2
   ТемператураAfter cooled
3. 3
   Другоеthe reaction liquid
4. 4
   Экстракцияextracted with chloroform
5. 5
   Сушкаthe organic layer was dried with anhydrous magnesium sulfate
6. 6
   Другоеthe solvent was evaporated away under reduced pressure
7. 7
   ДругоеThe resulting residue was purified
8. 8
   Другоеthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1)

Методика

20 mg of 2-mercaptoethanol and 10 mg of potassium carbonate were added in order to an N,N-dimethylformamide (1 ml) solution of 20 mg of 6-(1-acetylpyrrolidin-2-yl)-5-(6-chloropyridin-3-yl)oxy-2-pyridin-2-yl-1H-benzimidazole obtained in Example 504, and the reaction liquid was stirred at 120° C. for 5 hours. After cooled, the reaction liquid was diluted with aqueous saturated sodium bicarbonate, extracted with chloroform, and the organic layer was dried with anhydrous magnesium sulfate, and the solvent was evaporated away under reduced pressure. The resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1) to obtain the entitled compound as a white solid.

Источник