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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 557291Generated: October 29, 2026

Citric Acid → HCID 25070440, compound

https://huagongshe.com/reaction/557291

Reaction equation

Participants

RoleNameHCIDCharge
ReactantCitric AcidHCID 311—
ReactantMethanolHCID 887—
ReactantE-1210HCID 16719049—
Solventtert-Butyl methyl etherHCID 15413—
ProductHCID 25070440HCID 2507044087.2%

Reaction Conditions

Temperature32.5 °C

Reaction Steps

To 3-(3-(4-(pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-yl amine (1 g) and citric acid (564 mg) was added methanol (3 mL), and the suspension was stirred at 30 to 35° C, to turn it into a solution. Under stirring at 30° C, after adding tert-butyl methyl ether (3 mL) dropwise over 15 minutes to this solution and seeding, crystals precipitated. After stirring at 30° C for 10 minutes, tert-butyl methyl ether (15 mL) was added at the same temperature for one hour, and after slow cooling, mixture was stirred at 23° C for two hours. The precipitated crystals were filtered and dried to obtain the title compound (1.34 g) as a white crystal.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08058444B2
Source datasetuspto-grants-2011_11
ORD IDord-6016b34a1d3f420987ce5153f8c27450
Source noteuspto-grants-2011_11