Реакция #5301

Уравнение реакции

sodium hydride

2-chloro-4-(3-trifluoromethylphenoxy)phenol

2-chloro-5-chloromethylpyridine

→

2-chloro-5-[2-chloro-4-(3-trifluoromethylphenoxy)phenoxy]methylpyridine

Растворители

N,N-dimethylformamide

N,N-dimethylformamide

N,N-dimethylformamide

Условия реакции

Обработка

1. 1
   Температураice-cooling
2. 2
   Другоеat room temperature
3. 3
   workup.STIRRINGby stirring at the same temperature for 10 hours
4. 4
   Экстракцияextracted twice with 100 ml of ethyl acetate
5. 5
   Сушкаdried over anhydrous magnesium sulfate
6. 6
   Концентрированиеconcentrated under reduced pressure

Методика

To a solution 0.07 g of sodium hydride (60% oil dispersion) in 10 ml of N,N-dimethylformamide, there was added dropwise a solution of 0.50 g of 2-chloro-4-(3-trifluoromethylphenoxy)phenol in 3 ml of N,N-dimethylformamide with stirring and ice-cooling. After 30 minutes, a solution of 0.28 g of 2-chloro-5-chloromethylpyridine in 5 ml of N,N-dimethylformamide was added thereto at room temperature, followed by stirring at the same temperature for 10 hours. The reaction mixture was poured into ice-water and extracted twice with 100 ml of ethyl acetate. The extracts were combined together, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 2-chloro-5-[2-chloro-4-(3-trifluoromethylphenoxy)phenoxy]methylpyridine.

Источник