N,N'-Dimethylethylenediamine → HCID 57640611, compound

Participants

Role	Name	HCID	Charge
Reactant	N,N'-Dimethylethylenediamine	HCID 8070	—
Reactant	Potassium Phosphate, Tribasic	HCID 62657	—
Reactant	HCID 57640755	HCID 57640755	—
Reactant	HCID 178516071	HCID 178516071	—
Catalyst	Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)	HCID 24350	—
Solvent	Dimethyl Sulfoxide	HCID 679	—
Solvent	1,4-Dioxane	HCID 31275	—
Product	HCID 57640611	HCID 57640611	—

Reaction Conditions

Temperature	120 °C

Reaction Steps

Aryl iodide (Example 288, 43 mg, 0.1 mmol) and 2-hydroxypyridine (38 mg, 0.4 mmol) were dissolved in 1.2 mL dry dioxane and 0.5 mL dry DMSO in a sealed tube. To it were added N,N′-dimethylethylenediamine (11 μL, 0.1 mmol), CuI (10 mg, 0.05 mmol) and K3PO4 (42 mg, 0.2 mmol) in order. The mixture was stirred and heated in 120° C. bath for 6 hrs. The mixture was filtered and directly subjected to reverse phase preparative HPLC to isolate the title compound as a white powder after lyophilization. MS found for C20H14ClN3O3S as (M+H)+ 412.0, 414.0

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US08377974B2
Source dataset	uspto-grants-2013_02
ORD ID	ord-5ab8ca96397a499bbc431d1a4e201f32
Source note	uspto-grants-2013_02