反応 #90761

反応方程式

2,5-dichloro-4-iodopyridine

2-amino-N-methylbenzamide

tripotassium phosphate

Bis(2-diphenylphosphinophenyl)ether

→

product

収率 56.5%

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

収率 56.5%

溶媒

1,4-dioxane

反応条件

後処理

1. 1
   その他A 150-mL sealed tube
2. 2
   その他The reaction mixture was degassed with nitrogen for 10 min
3. 3
   ろ過The reaction mixture was filtered through celite, which
4. 4
   洗浄was washed with dioxane
5. 5
   その他The solvent was evaporated to dryness
6. 6
   洗浄the solid was washed with EtOH (10 mL×3)

実験手順

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.

出典