Potassium Phosphate, Tribasic → HCID 86668805, compound

Participants

Role	Name	HCID	Charge
Reactant	Potassium Phosphate, Tribasic	HCID 62657	—
Reactant	5-Chloro-2-nitroanisole	HCID 81110	—
Reactant	1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)	HCID 636044	—
Reactant	Diethylphosphite	HCID 3780918	—
Catalyst	palladium(II) acetate	HCID 167845	—
Solvent	Dimethylformamide	HCID 6228	—
Product	HCID 86668805	HCID 86668805	33%

Reaction Steps

To a solution of 5-chloro-2-nitroanisole (1.00 g, 5.33 mmol) in 20 mL DMF was added diethyl phosphite (0.809 g, 5.86 mmol), palladium acetate (0.060 g, 0.27 mmol), XANTPHOS (0.185 g, 0.320 mmol), and potassium phosphate (1.24 g, 5.86 mmol). The mixture was purged with nitrogen, and subjected to microwaves at 150° C. for 20 minutes. The reaction mixture was concentrated and purified by silica gel chromatography (0-45% ethyl acetate:heptane) to afford the desired product (0.504 g, 33% yield).

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US09273077B2
Source dataset	uspto-grants-2016_03
ORD ID	ord-5e8f2ad2f45f451ebfb3b8c15d51a186
Source note	uspto-grants-2016_03