1,4-Dioxane hydrochloride → N,N-bis(1H-imidazol-2-ylmethyl)-N'-(piperidin-4-ylmethyl)urea

Participants

Role	Name	HCID	Charge
Reactant	1,4-Dioxane hydrochloride	HCID 20443148	—
Reactant	tert-butyl 4-[({[bis({1-[(dimethylamino)sulfonyl]-1H-imidazol-2-yl)methyl]amino}carbonyl)amino]methyl}piperidine-1-carboxylate	HCID 67500244	—
Product	N,N-bis(1H-imidazol-2-ylmethyl)-N'-(piperidin-4-ylmethyl)urea	HCID 67502645	—

Reaction Conditions

Temperature	60 °C

Reaction Steps

To the compound (3.00 g) obtained in Example 9, 4N hydrogen chloride/dioxane (15 mL) was added. The reaction solution was stirred at 60° C. for 15 hours. The reaction solution was concentrated under reduced pressure. The residue was dissolved in methanol (20 mL) and a carbonate resin (trade name: MP-Carbonate, manufactured by Argonaut Co., product number: 800267, 10 g) was added, followed by stirring at room temperature for 3 hours. After the resin was removed by filtration, the filtrate was concentrated under reduced pressure. The title compound was obtained without purifying the residue.

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US08519124B2
Source dataset	uspto-grants-2013_08
ORD ID	ord-9c00655d02874f19a712a819e4343779
Source note	uspto-grants-2013_08