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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 841080Generated: November 1, 2026

Tri-o-tolylphosphine → 5'-Ethenylspiro[1-azabicyclo[2.2.2]octane-3,2'(3'H)-furo[2,3-b]pyrdine]

https://huagongshe.com/reaction/841080

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTri-o-tolylphosphineHCID 80271—
ReactantLithium ChlorideHCID 433294—
Reactant5'-bromospiro[1-azabicyclo[2.2.2]octane-3,2'(3'H)-furo[2,3-b]pyridine]HCID 10357133—
ReactantTri(butyl)vinylstannaneHCID 21115800—
SolventMethanolHCID 887—
SolventChloroformHCID 6212—
Solvent1,2-DimethoxyethaneHCID 8071—
Product5'-Ethenylspiro[1-azabicyclo[2.2.2]octane-3,2'(3'H)-furo[2,3-b]pyrdine]HCID 22045864186.9%

Reaction Steps

A solution containing 5′-bromospiro[1-azabicyclo[2.2.2]octane-3,2′(3′H)-furo[2,3-b]pyridine] (150 mg, 0.508 mmol), tris(dibenzylidineacetone)dipalladium (0) (22 mg, 0.024 mmol), tri(o-tolyl)phosphine (63 mg, 0.206 mmol), lithium chloride (103 mg, 2.43 mmol), and tri-n-butylvinylstannane (188 mg, 0.592 mmol) in 1,2-dimethoxyethane (10 ml) was heated under reflux overnight. The solution was evaporated, and the residue was taken up in chloroform and filtered. The filtrate was evaporated then purified by HPLC using a gradient of 0-25% 1:1:2 7M methanolic ammonia:methanol:chloroform and chloroform to obtain the title compound (93 mg, 0.385 mmol, 76%) as a pale solid: electrospray MS (m/z, relative intensity) 243 ([MH]+, 100).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06369224B1
Source datasetuspto-grants-2002_04
ORD IDord-5b58ca1899ba4b66a8e5779410202a99
Source noteuspto-grants-2002_04