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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 341026Generated: October 31, 2026

Tributyltin Chloride → HCID 68159442, compound

https://huagongshe.com/reaction/341026

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTributyltin ChlorideHCID 15096—
ReactantThiazole, 5-(2-thienyl)-HCID 11217456—
ReactantHCID 131731282HCID 131731282—
ReactantButyllithiumHCID 178418339—
SolventDiethyl EtherHCID 3283—
SolventDimethylformamideHCID 6228—
ProductHCID 68159442HCID 68159442—

Reaction Conditions

Temperature-78 °C

Reaction Steps

A solution of 5-(2-thienyl)thiazole (0.4 mmol) in diethyl ether was cooled to −78° C., and n-butyllithium (0.4 mmol, 1.57 M solution in hexane) was added thereto, followed by stirring at −78° C. for 30 min. Furthermore, tributylstannyl chloride was added thereto, followed by stirring at room temperature for 30 min. The reaction solution was separated between ethyl acetate and water. The organic layer was washed with saturated brine and concentrated, and 1-[2-deoxy-3,5-di-O-(toluoyl)-β-D-ribofuranosyl]-4-iodo-pyrrolo[2,3-b]pyridine (120 mg, 0.2 mmol), chlorobistriphenylphosphine palladium (5% mol), and DMF (2 mL) were added thereto, followed by stirring at 100° C. for 1 hr. The reaction solution was separated between ethyl acetate and water, and the organic layer was washed with saturated brine and water, dried over anhydrous sodium sulfate, and concentrated. After purification with a silica gel column and addition of sodium methoxide (1.6 mL), the resulting mixture was stirred at room temperature for 30 min. dDvas nucleoside (34 mg) was purified with a silica gel column and by HPLC.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08895712B2
Source datasetuspto-grants-2014_11
ORD IDord-fdfcb3c5cd1648acbea3de5be205b063
Source noteuspto-grants-2014_11