Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1508618Generated: October 31, 2026

Methanol → HCID 89975735, compound

https://huagongshe.com/reaction/1508618

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethanolHCID 887—
Reactantp-Xylyl bromideHCID 7721—
ReactantSodium hydrideHCID 24758—
ReactantHCID 20768265HCID 20768265—
SolventDimethylformamideHCID 6228—
ProductHCID 89975735HCID 8997573584.3%

Reaction Steps

In a nitrogen atmosphere, 0.44 g of sodium hydride and 2.03 g of 4-methylbenzyl bromide were added to a solution of 0.70 g of (2R,3R,4S)-4-fluoro-2-(hydroxymethyl)-5-methoxyoxolan-3-ol in 7.0 mL of N,N-dimethylformamide under cooling on ice, and the obtained mixture was then stirred at room temperature for 2 hours. Thereafter, 2.5 mL of methanol was added to the reaction mixture to terminate the reaction, and ethyl acetate and hexane were then added thereto. The reaction mixture was successively washed with water and a saturated sodium chloride aqueous solution, and was then dried over anhydrous magnesium sulfate. After that, the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=90/10 to 60/40), so as to obtain 1.33 g of (3S,4R,5R)-3-fluoro-2-methoxy-4-((4-methylbenzyl)oxy)-5-(((4-methylbenzyl)oxy)methyl)oxolane in the form of a colorless oily product.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09221865B2
Source datasetuspto-grants-2015_12
ORD IDord-55db92ebdff143598e8cbd6263a37a29
Source noteuspto-grants-2015_12