Tetrahydrofuran → HCID 178473742, compound

Participants

Role	Name	HCID	Charge
Reactant	Tetrahydrofuran	HCID 8028	—
Reactant	Triethylamine	HCID 8471	—
Reactant	4-Amino-1-methylpiperidine	HCID 2737531	—
Reactant	1-[2,6-Dichloro-8-(3-chloro-4-fluorophenylamino)-4H-pyrimido[5,4-d]pyrimidin-3-yl]ethanone	HCID 22592970	—
Solvent	Water	HCID 962	—
Product	HCID 178473742	HCID 178473742	—

Reaction Conditions

Temperature	50 °C

Reaction Steps

47.2 g (0.413 mol) of 1-methyl-4-aminopiperidine is added dropwise at ambient temperature to a mixture of 123.3 g (0.317 mol) of (3), 740 ml of THF and 61.7 ml (0.445 mol) of triethylamine. The mixture is stirred for 30 min at 50° C. It is left to cool to 40° C., 1480 ml of water are added and the mixture is then stirred for 90 minutes at 10° C. The product that crystallises out is filtered off, washed with 150 ml of water and dried in vacuo at 60° C. The product is dissolved in 1150 ml of ethyl acetate at boiling temperature. It is cooled to 10° C., filtered and the product that crystallises out is dried at 60° C. in vacuo. Yield: 128.9 g (87.2%).

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US06849734B2
Source dataset	uspto-grants-2005_02
ORD ID	ord-06a7203e45974abea770c02cd055dcd5
Source note	uspto-grants-2005_02