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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2202516Generated: November 2, 2026

Methanol → HCID 67387130, compound

https://huagongshe.com/reaction/2202516

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethanolHCID 887—
ReactantSulfuric AcidHCID 1118—
Reactant3-(2,5-Dimethyl-pyrrol-1-yl)-6-methoxy-5-trifluoromethyl-pyridine-2-carboxylic acidHCID 58442313—
ProductHCID 67387130HCID 67387130—

Reaction Steps

3-(2,5-Dimethyl-pyrrol-1-yl)-6-methoxy-5-trifluoromethyl-pyridine-2-carboxylic acid (Intermediate D2) (500 mg, 1.591 mmol) in methanol (15.91 ml) was treated with H2SO4 (0.0424 ml, 0.795 mmol) and the soltuion was heated at reflux for overnight. The solvent removed was removed in vacuo and the resulting brown oil was neutralised to pH 7 using saturated sodium bicarbonate. The mixture was extracted with EtOAc (20 ml) and the combined organic extracts were washed with water (20 ml), brine (20 ml), passed though a phase separator and concentrated in vacuo. Purification of the crude product by chromatography on silica eluting with iso-hexane: EtOAc (gradient of 0 to 10% EtOAc) afforded the title compound as an off-white powder.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09365552B2
Source datasetuspto-grants-2016_06
ORD IDord-ae7a6888d366422f897f4316ecc8ffc9
Source noteuspto-grants-2016_06