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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 911557Generated: October 31, 2026

Water → HCID 57656392, compound

https://huagongshe.com/reaction/911557

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantHCID 57655903HCID 57655903—
ReactantHCID 86761413HCID 86761413—
CatalystCopper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)HCID 24350—
SolventEthyl AcetateHCID 8857—
SolventN-methyl-2-pyrrolidoneHCID 13387—
ProductHCID 57656392HCID 5765639274%

Reaction Conditions

Temperature180 °C

Reaction Steps

To a stirred solution of 7-bromo-6-dimethylcarbamoylthio-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (1.383 g, 3.254 mmol), in NMP (40 ml) add sodium trifluoromethyl acetate (3.54 g, 26.03 mmol), copper(I) iodide (2.47 g, 13.0 mmol) and heat the mixture at 180° C. for 4 h. Cool to ambient temperature. Dilute with EtOAc, water and remove the copper solid residue by filtration. Separate the layers of filtrate and extract the aqueous layer three times with EtOAc. Dry over anhydrous Na2SO4, and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (6:1) to give the desired intermediate as a yellow oil (882 mg, 74%).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08022062B2
Source datasetuspto-grants-2011_09
ORD IDord-26657f34978d47fd9342c77094ba23b6
Source noteuspto-grants-2011_09