Sodium hydride → (8S)-9-[(2,4-difluorophenyl)carbonyl]-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetra-hydro-4 H-pyrimido[1,2-a]pyrimidin-4-one

Beteiligte Stoffe

Rolle	Name	HCID	Einwaage
Edukt	Sodium hydride	HCID 24758	—
Edukt	2,4-Difluorobenzoyl chloride	HCID 588081	—
Edukt	Dichloromethane methanol	HCID 21226129	—
Edukt	(S)-8-(Morpholin-4-yl)-2-(trifluoromethyl)-1,2,3,4-tetrahydropyrimido[1,2-a]pyrimidin-6-one	HCID 136238743	—
Lösungsmittel	Tetrahydrofuran	HCID 8028	—
Produkt	(8S)-9-[(2,4-difluorophenyl)carbonyl]-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetra-hydro-4 H-pyrimido[1,2-a]pyrimidin-4-one	HCID 49854504	5,5%

Reaktionsschritte

The product is prepared according to the procedure described in Example 18, using 300 mg of (8S)-2-morpholin-4-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one (Example 1e), 47 mg of sodium hydride and 174 mg of 2,4-difluorobenzoyl chloride in 4 ml of tetrahydrofuran. After two successive purifications by silica chromatography (eluent: CH2Cl2/MeOH, gradient of 100/0 to 98/02 then 99/01), 24 mg of (8S)-9-[(2,4-difluorophenyl)carbonyl]-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetra-hydro-4 H-pyrimido[1,2-a]pyrimidin-4-one are obtained in the form of a colourless lacquer, the characteristics of which are the following:

Herkunft & Nachweise

DOI	10.6084/m9.figshare.5104873.v1
Patentnummer	US08846670B2
Quelldatensatz	uspto-grants-2014_09
ORD ID	ord-4125b8d2c6b4412a85323a959139f6c6
Quellennotiz	uspto-grants-2014_09