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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 879993Generated: October 25, 2026

Water → 1,1-dimethylethyl 7-(3-{[(4-methyl-2-pyridinyl)methyl]oxy}-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate

https://huagongshe.com/reaction/879993

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantCesium carbonateHCID 10796—
Reactanttert-Butyl 7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,4,5-tetrahydro-3H-benzo[d]azepine-3-carboxylateHCID 57505869—
Reactant2-Bromo-3-{[(4-methyl-2-pyridinyl)methyl]oxy}pyridineHCID 86670544—
CatalystPalladium ChlorideHCID 24290—
CatalystFerrocene-1,1'-bis-(diphenylphosphine)HCID 635956—
SolventEthyl AcetateHCID 8857—
Solvent1,4-Dioxane--water (1/1)HCID 21886435—
Product1,1-dimethylethyl 7-(3-{[(4-methyl-2-pyridinyl)methyl]oxy}-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylateHCID 70665243—

Reaction Conditions

Temperature120 °C

Reaction Steps

To a degassed mixture of 2-bromo-3-{[(4-methyl-2-pyridinyl)methyl]oxy}pyridine (2.83 g), 1,1-dimethylethyl 7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (4.54 g) and cesium carbonate (9.9 g) in dioxane:water (4:1, 40 ml) was added PdCl2.dppf (0.828 g). The reaction mixture was heated at 120° C. overnight. The reaction mixture was added to water and extraction was carried out with ethyl acetate. The organic layer was dried over sodium sulphate and the filtrate was concentrated in vacuo. The crude product was purified through silica, eluting with 0-40% ethyl acetate in hexane. Appropriate fractions were concentrated in vacuo to yield the title compound, 3.8 g (84%).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08993560B2
Source datasetuspto-grants-2015_03
ORD IDord-806a556025984cc58feff664d5c4ebd7
Source noteuspto-grants-2015_03