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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 520407Generated: October 29, 2026

Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 86690117, compound

https://huagongshe.com/reaction/520407

Reaction equation

Participants

RoleNameHCIDCharge
ReactantBenzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 466102—
ReactantHCID 86690116HCID 86690116—
SolventAcetoneHCID 180—
SolventWaterHCID 962—
SolventEthyl AcetateHCID 8857—
ProductHCID 86690117HCID 8669011785%

Reaction Conditions

Temperature60 °C

Reaction Steps

To a solution of ethyl (1S)-6-oxospiro[2.5]octane-1-carboxylate (1.9 g, 7.91 mmol) in acetone (20 mL) and water (5 mL) was added PPTS (0.1 g, 0.398 mmol). The reaction mixture was heated at 60° C. for 5 h, and then stirred at rt for 45 h. The reaction mixture was diluted with EtOAc, washed with water, brine, dried (MgSO4) and concentrated to afford ethyl 6-oxospiro[2.5]octane-1-carboxylate as an oil (1.32 g). 1H NMR (400 MHz, CDCl3) δ ppm 4.13-4.21 (2H, m), 2.35-2.51 (3H, m), 2.19-2.30 (1H, m), 2.00-2.09 (3H, m), 1.86 (1H, ddd, J=13.68, 8.16, 5.27 Hz), 1.64-1.77 (2H, m), 1.23-1.35 (3H, m), 1.08 (1H, dd, J=8.16, 4.64 Hz).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09326973B2
Source datasetuspto-grants-2016_05
ORD IDord-3b40d98295d5475ea63a34a119964709
Source noteuspto-grants-2016_05