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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1699397Generated: October 29, 2026

Water → HCID 18319519, compound

https://huagongshe.com/reaction/1699397

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantEthyl AcetateHCID 8857—
ReactantDimethyl DisulfideHCID 12232—
ReactantHCID 18319622HCID 18319622—
SolventAcetonitrileHCID 6342—
ProductHCID 18319519HCID 18319519—

Reaction Conditions

Temperature50 °C

Reaction Steps

The mixture of ethyl 2,3-dihydro-7-amino-1-benzoxepin-4-carboxylate (2.0 g), dimethyl disulfide (2.3 ml) and t-butylnitrile (1.2 ml) in acetonitrile (4 ml) was stirred at 50° C. for 2.5 hours. The mixture was poured into a mixture of ethyl acetate and water. The separated organic layer was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel using a mixture of hexane and toluene (1:1) as an eluent. The eluted fractions containing the desired product were collected and evaporated in vacuo to give ethyl 2,3-dihydro-7-methylthio-1-benzoxepin-4-carboxylate (1.24 g).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06346527B1
Source datasetuspto-grants-2002_02
ORD IDord-373bff12358e4be6bda83cc70755305c
Source noteuspto-grants-2002_02