Cesium carbonate → (2-Bromo-6-{4,4-dimethyl-9-oxo-7-thia-10-azatricyclo[6.4.0.02,6]dodeca-1(8),2(6)-dien-10-yl}-4-fluorophenyl)methyl Acetate

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	6,6-Dimethyl-2,3,4,5,6,7-hexahydro-1H-cyclopenta[4,5]thieno[2,3-c]pyridin-1-one	HCID 58043895	—
반응물	2,6-Dibromo-4-fluorobenzyl acetate	HCID 67016593	—
촉매	Bis(dibenzylideneacetone)palladium	HCID 9811564	—
용매	1,4-Dioxane	HCID 31275	—
생성물	(2-Bromo-6-{4,4-dimethyl-9-oxo-7-thia-10-azatricyclo[6.4.0.02,6]dodeca-1(8),2(6)-dien-10-yl}-4-fluorophenyl)methyl Acetate	HCID 58044256	71.1%

반응 조건

온도	100 °C

반응 단계

A mixture of 113h (2 g, 9.05 mmol), 2,6-dibromo-4-fluorobenzyl acetate (101j)(8.8 g, 27.15 mmol), XantPhos (524 mg, 0.9 mmol), Pd2(dba)3 (828 mg, 0.9 mmol) and Cs2CO3 (5.9 g, 18 mmol) in dioxane (200 mL) was heated at 100° C. for 15 h under nitrogen. The reaction mixture was filtered and the filtrated was evaporated in vacuo. The residue was purified by silical-gel column eluting with 1:1 ethyl acetate/petroleum ether to give 113i as a yellow solid (3 g, 71%). MS: (M+H)+ 466.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08722676B2
출처 데이터셋	uspto-grants-2014_05
ORD ID	ord-9495e1aa2a6a4d7092030ca832ee317e
출처 메모	uspto-grants-2014_05