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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 658095Generated: October 26, 2026

Ammonium Chloride → HCID 68451303, compound

https://huagongshe.com/reaction/658095

Reaction equation

Participants

RoleNameHCIDCharge
ReactantAmmonium ChlorideHCID 25517—
ReactantMethyltriphenylphosphonium iodideHCID 638159—
ReactantHCID 86626216HCID 86626216—
ReactantHCID 178420697HCID 178420697—
SolventTetrahydrofuranHCID 8028—
ProductHCID 68451303HCID 6845130350%

Reaction Conditions

Temperature0 °C

Reaction Steps

At −78° C., 9.50 ml of 1.59 M n-butyl lithium-THF solution was added dropwise to 90 ml of THF solution containing 8.13 g of methyltriphenylphosphonium iodide. This was stirred at 0° C. for 10 minutes, cooled to −78° C. and then mixed with 2.44 g of tert-butyl 2,4-difluoro-3-formylbenzoate dissolved in 10 ml of THF. After 40 minutes thereof, this was stirred at room temperature for 1 hour, mixed with appropriate amounts of saturated ammonium chloride aqueous solution and purified water, extracted with ethyl acetate and then dried with anhydrous magnesium sulfate. After concentration, the thus formed residue was purified by a silica gel column chromatography to obtain 1.20 g (50%) of tert-butyl 2,4-difluoro-3-vinylbenzoate (Reference Example 5-1) from a hexane-ethyl acetate (50:1) eluate. ES−: 239

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08076367B2
Source datasetuspto-grants-2011_12
ORD IDord-d3424850e7084df9b99bb89841dd8669
Source noteuspto-grants-2011_12