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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1253593Generated: November 2, 2026

Isopropanol → HCID 59367711, compound

https://huagongshe.com/reaction/1253593

Reaction equation

Participants

RoleNameHCIDCharge
ReactantIsopropanolHCID 3776—
ReactantAmmonium ChlorideHCID 25517—
ReactantBenzoic acid, 4-fluoro-, ethyl esterHCID 67976—
Reactant4-MethylpyridazineHCID 136882—
ReactantSodium hexamethyidisilazaneHCID 45051731—
SolventDiisopropyl EtherHCID 7914—
SolventTetrahydrofuranHCID 8028—
ProductHCID 59367711HCID 5936771177.5%

Reaction Conditions

Temperature0 °C

Reaction Steps

A solution under argon of 1.88 g (20.0 mmol) of 4-methylpyridazine and 3.36 g (20.0 mmol) of ethyl 4-fluorobenzoate in 50 ml of anhydrous tetrahydrofuran is cooled to 0° C. and then 20.0 ml (40.0 mmol) of a 2M solution of sodium hexamethyldisilazane in tetrahydrofuran (THF) are added dropwise. After the addition, the temperature is allowed to return to ambient temperature, while a gradual setting of the reaction medium is observed. After one hour, the mixture is poured into an aqueous solution of ammonium chloride and the product is extracted with ethyl acetate. The organic phase is dried over sodium sulfate, filtered and concentrated under reduced pressure to give an orangey-red solid. The latter is triturated at reflux in 80 ml of diisopropyl ether containing a few ml of isopropyl alcohol and the solid is then isolated by filtration after cooling to 0° C. 3.35 g of a pale yellow powder are thus isolated after drying.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08455491B2
Source datasetuspto-grants-2013_06
ORD IDord-43ac315c1b114ae19ad6879d0686949a
Source noteuspto-grants-2013_06