Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1169445Generated: November 3, 2026

Triphenylphosphine → HCID 22990048, compound

https://huagongshe.com/reaction/1169445

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTriphenylphosphineHCID 11776—
Reactantethyl N-ethoxycarbonyliminocarbamateHCID 220568—
ReactantMethyl 7-hydroxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylateHCID 22989977—
ReactantHCID 70023923HCID 70023923—
SolventTolueneHCID 1140—
SolventTetrahydrofuranHCID 8028—
ProductHCID 22990048HCID 22990048151.5%

Reaction Steps

Into a solution of methyl 7-hydroxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (400 mg), 2-(2-propoxyethoxy)benzyl alcohol (0.63 g) and triphenylphosphine (782 mg) in THF (10 ml) was added at 0° C. diethyl azodicarboxylate (a 40% solution in toluene, 1.36 ml), and the resulting mixture was stirred at room temperature for 20 hours. After concentration under reduced pressure, the residue was subjected to separation and purification using column chromatography (ethyl acetate/hexane 1:2) to obtain crude methyl 7-[[2-(2-propoxyethoxy)benzyl]oxy]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (1.04 g).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06627651B1
Source datasetuspto-grants-2003_09
ORD IDord-65b6d8280d1d4d59b6fddb363faf686d
Source noteuspto-grants-2003_09