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26483-64-7

PHENYLPYRIDYLMETHYL ACETATE synthesis

7synthesis methods
-

Yield:26483-64-7 97%

Reaction Conditions:

with palladium diacetate;caesium carbonate;XPhos in 1,4-dioxane at 100; for 12 h;Inert atmosphere;Schlenk technique;

Steps:

1.2 General procedure for the arylation reaction

General procedure: An oven-dried Schlenk tube was charged with Pd(OAc)2 (0.015 mmol, 3.4 mg), X-Phos (0.015 mmol, 7.2 mg), Cs2CO3 (0.9 mmol, 293 mg), substrate 1 (0.3 mmol) and 2 (0.4 mmol). The reaction vessel was evacuated and backfilled again with nitrogen gas, and 1,4-dioxane (1 mL) was added via syringe under nitrogen. The reaction mixture was stirred at 100 °C for 12 hours. The reaction mixture was then cooled to room temperature and diluted with EtOAc. The crude was nextfiltered through a plug of celite, which was washed with ethyl acetate. The solution was concentrated and further purifiedby flash column chromatography to afford the corresponding product.

References:

Jin, Chaochao;Xu, Kun;Fan, Xiao;Liu, Changyao;Tan, Jiajing [Chinese Chemical Letters,2020,vol. 31,# 1,p. 91 - 94] Location in patent:supporting information