Cesium carbonate → 6-Bromo-4-(2-tert-butyl-5-methyl-2H-pyrazol-3-ylamino)-2-(4-tert-butyl-phenyl)-2H-phthalazin-1-one

참여 물질

역할	이름	HCID	투입량
반응물	Cesium carbonate	HCID 10796	—
반응물	1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)	HCID 636044	—
반응물	1-tert-Butyl-3-methyl-1H-pyrazol-5-amine	HCID 737200	—
반응물	HCID 21106542	HCID 21106542	—
촉매	Bis(dibenzylideneacetone)palladium	HCID 9811564	—
생성물	6-Bromo-4-(2-tert-butyl-5-methyl-2H-pyrazol-3-ylamino)-2-(4-tert-butyl-phenyl)-2H-phthalazin-1-one	HCID 21106578	194.9%

반응 조건

온도	100 °C

반응 단계

11 mg 4,6-Dibromo-2-(4-tert-butyl-phenyl)-2H-phthalazin-1-one (preparation see ZA-1) were reacted with 39.0 mg 1-tert.-butyl-3-methyl-1H-pyrazol-5-ylamine, 132 mg cesium carbonate, 7.0 mg tris-(dibenzylideneacetone)-dipalladium and 8.8 mg 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene were stirred under argon at 100° C. for 20 hrs until HPLC indicated complete conversion. The solvent was removed under vacuum, the residue was taken up in DCM and washed dilute HCl. Removal of the DCM and chromatography on silica in first heptane and then heptan/EtOAc 8:2 yielded 25 mg of the title product.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US07501410B2
출처 데이터셋	uspto-grants-2009_03
ORD ID	ord-c316b6106d424f979bd720905c4400ca
출처 메모	uspto-grants-2009_03