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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2078820Generated: November 1, 2026

Acetamide → 8-acetamido-N-(2-chloro-4-(4-methylpiperazine-1-carbonyl)phenyl)-N-methyl-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamide

https://huagongshe.com/reaction/2078820

Reaction equation

Participants

RoleNameHCIDCharge
ReactantAcetamideHCID 178—
ReactantCesium carbonateHCID 10796—
Reactant1,4-DioxaneHCID 31275—
Reactant1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 636044—
Reactant8-bromo-N-(2-chloro-4-(4-methylpiperazine-1-carbonyl)phenyl)-N-methyl-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamideHCID 56834369—
CatalystBis(dibenzylideneacetone)palladiumHCID 9811564—
Product8-acetamido-N-(2-chloro-4-(4-methylpiperazine-1-carbonyl)phenyl)-N-methyl-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamideHCID 579002255.5%

Reaction Conditions

Temperature100 °C

Reaction Steps

Following the procedure of Example 91, to a solution containing 8-bromo-N-(2-chloro-4-(4-methylpiperazine-1-carbonyl)phenyl)-N-methyl-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamide (0.095 g, 0.16 mmol) in 1,4-dioxane (2.00 mL, 25.6 mmol) was added 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (XantPhos, 9.6 mg, 0.016 mmol), acetamide (15 mg, 0.25 mmol), and cesium carbonate (120 mg, 0.36 mmol) then degassed with nitrogen gas for 15 min. To the reaction mixture was added tris(dibenzylideneacetone)dipalladium(0) (Pd2(dba)3, 7.6 mg, 0.0083 mmol). The reaction mixture was heat at 100° C. for 18 h. The crude product was submitted for rHPLC to give 147 (5.5%). MS: (ESI+) 553.2

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07928248B2
Source datasetuspto-grants-2011_04
ORD IDord-33f7eec43970465d918cae8c3d7a2f2d
Source noteuspto-grants-2011_04