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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1015982Generated: October 31, 2026

Sodium Bicarbonate → HCID 59556098, compound

https://huagongshe.com/reaction/1015982

Reaction equation

Participants

RoleNameHCIDCharge
ReactantSodium BicarbonateHCID 516892—
ReactantEthyl acetate hexaneHCID 21226206—
ReactantHCID 59556067HCID 59556067—
SolventHydrochloric AcidHCID 313—
SolventTetrahydrofuranHCID 8028—
ProductHCID 59556098HCID 59556098118.4%

Reaction Conditions

Temperature60 °C

Reaction Steps

4-(8-Hydroxy-1,4-dioxaspiro[4.5]dec-8-yl)-N-methylbenzamide (410 mg, 1.4 mmol) was dissolved in the mixture solvent of 7 mL of THF and 7 mL of 1 N HCl aqueous solution at room temperature. The reaction mixture was then stirred at 60° C. for 1 h. The solution was cooled down to room temperature, adjusted to pH 7-8 with saturated NaHCO3 aqueous solution. The organic layer was separated, and the aqueous layer was extracted twice with EA (20 mL×2). The combined organic extracts were dried over MgSO4 and evaporated to give an oil residue. Chromatography on silica gel (flash chromatography grade) with 40% Ethyl acetate-hexane gave 410 mg (90%) of the desired product: 1H NMR (CDCl3) δ 7.78 (2H, d, J=11.2 Hz), 7.51 (2H, d, J=10.9 Hz), 4.10 (H, s), 3.37 (3H, s), 2.79-2.74 (2H, m), 2.63-2.49 (2H, m), 1.95-1.89 (2H, m), 1.67-1.59 (2H, m); MS: 248 (M+1)+.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07985730B2
Source datasetuspto-grants-2011_07
ORD IDord-a234e12f90ae422483d2a0188f986363
Source noteuspto-grants-2011_07