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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2046726Generated: November 2, 2026

Picolyl chloride hydrochloride → HCID 66932235, compound

https://huagongshe.com/reaction/2046726

Reaction equation

Participants

RoleNameHCIDCharge
ReactantPicolyl chloride hydrochlorideHCID 23392—
Reactant(E)-3-{1'-tert-butoxycarbonyl-4-oxo-spiro[chromane-2,4'-piperidine]-6-yl}-acrylic acid methyl esterHCID 52952087—
SolventDichloromethaneHCID 6344—
ProductHCID 66932235HCID 6693223578.8%

Reaction Steps

A suspension of (E)-3-{4-oxo-spiro[chromane-2,4′-piperidine]-6-yl}-acrylic acid methyl ester hydrochloride (150 mg, 0.44 mmol, Intermediate 1) in DCM (7 ml) was treated with TEA (0.49 ml, 3.52 mmol) and 2-(chloromethyl)pyridine hydrochloride (145 mg, 0.89 mmol), and stirred at RT for 48 h. Catalytic amount of KI was added and the reaction was stirred at RT overnight. The mixture was then washed with water and brine, dried and concentrated. The crude residue was purified by column chromatography (eluent: DCM/MeOH/NH4OH 96:4:0.2) to give (E)-3-{1′-(pyridin-2-ylmethyl)-4-oxo-spiro[chromane-2,4′-piperidine]-6-yl}-acrylic acid methyl ester (136 mg).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08592444B2
Source datasetuspto-grants-2013_11
ORD IDord-60291cc90d3e46be82958dbae0959797
Source noteuspto-grants-2013_11