Реакция #90761

Уравнение реакции

2,5-dichloro-4-iodopyridine

2-amino-N-methylbenzamide

tripotassium phosphate

Bis(2-diphenylphosphinophenyl)ether

→

product

Выход 56.5%

2-[(2,5-Dichloro-4-pyridinyl)amino]-N-methylbenzamide

Выход 56.5%

Растворители

1,4-dioxane

Условия реакции

Обработка

1. 1
   ДругоеA 150-mL sealed tube
2. 2
   ДругоеThe reaction mixture was degassed with nitrogen for 10 min
3. 3
   ФильтрацияThe reaction mixture was filtered through celite, which
4. 4
   Промывкаwas washed with dioxane
5. 5
   ДругоеThe solvent was evaporated to dryness
6. 6
   Промывкаthe solid was washed with EtOH (10 mL×3)

Методика

A 150-mL sealed tube was charged with 2,5-dichloro-4-iodopyridine (3.5 g, 12.78 mmol), 2-amino-N-methylbenzamide (1.919 g, 12.78 mmol) and tripotassium phosphate (8.14 g, 38.3 mmol) in 1,4-dioxane (100 mL). The reaction mixture was degassed with nitrogen for 10 min. Bis(2-diphenylphosphinophenyl)ether (DPEPhos, 0.688 g, 1.278 mmol) and Pd(OAc)2 (0.115 g, 0.511 mmol) were added and the reaction mixture was heated in a 120° C. oil bath over night. The reaction mixture was filtered through celite, which was washed with dioxane. The solvent was evaporated to dryness and the solid was washed with EtOH (10 mL×3) to give 2.14 g (56%) of product as an off white solid.

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