Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1949718Generated: November 3, 2026

Acetamide → HCID 44242428, compound

https://huagongshe.com/reaction/1949718

Reaction equation

Participants

RoleNameHCIDCharge
ReactantAcetamideHCID 178—
ReactantCesium carbonateHCID 10796—
Reactant1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 636044—
Reactant8-bromo-N-(2-chlorophenyl)-N-methyl-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamideHCID 44242427—
Solvent1,4-DioxaneHCID 31275—
ProductHCID 44242428HCID 44242428—

Reaction Conditions

Temperature110 °C

Reaction Steps

To a suspension of 8-bromo-N-(2-chlorophenyl)-N-methyl-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamide 150 (100 mg, 0.22 mmol), Cs2CO3 (158 mg), acetamide (20 mg), and xantphos (13 mg) in dry 1,4-dioxane (2 mL) was degassed with bubbling N2. Pd2 dba3 was added and the 10 mL tube was sealed and heated at 110° C. for 8 hr. After cooling to room temp., the mixture was diluted with water and extracted with ethylacetate. The combined organics were concentrated and the crude residue obtained purified by reverse phase HPLC to give 151. 1H NMR (500 MHz, DMSO-d6) δ 10.03 (s, 1H), 7.65 (m, 2H), 7.62 (m, 2H), 7.35 (m, 2H), 7.17 (m, 1H), 6.51 (br s, 1H), 4.15 (m, 2H), 3.29 (s, 3H), 2.91 (m, 2H), 2.03 (s, 3H) MS: (ESI+) 427.1

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08399690B2
Source datasetuspto-grants-2013_03
ORD IDord-a84f8ae49cf1485bb3a98028c61b6128
Source noteuspto-grants-2013_03