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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1051984Generated: November 4, 2026

p-Toluenesulfonic acid monohydrate → Methyl 3-(4-oxopiperidin-1-yl)benzoate

https://huagongshe.com/reaction/1051984

Reaction equation

Participants

RoleNameHCIDCharge
Reactantp-Toluenesulfonic acid monohydrateHCID 521998—
ReactantMethyl-3-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)benzoateHCID 60059302—
SolventAcetoneHCID 180—
SolventWaterHCID 962—
ProductMethyl 3-(4-oxopiperidin-1-yl)benzoateHCID 6005932279.3%

Reaction Steps

A mixture of methyl-3-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)-benzoate (1.80 g, 6.49 mmol) and p-toluenesulfonic acid monohydrate (123 mg, 0.649 mmol) in water (30 mL) and acetone (15 mL) was heated at reflux for 17 hours. The organic solvent was removed in vacuo and the aqueous mixture was extracted with dichloromethane. The organic extract was washed with saturated NaHCO3(aq.), dried (MgSO4), filtered and concentrated. Elution through a flash column (silica gel 60, 230-400 mesh, 3:2 hexanes:EtOAc) followed by concentration gave the title compound as a yellow oil (1.20 g, 79%).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09388176B2
Source datasetuspto-grants-2016_07
ORD IDord-305e114f647749b1b006460427ae49b7
Source noteuspto-grants-2016_07