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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2358520Generated: October 31, 2026

Methanol → HCID 23078198, compound

https://huagongshe.com/reaction/2358520

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethanolHCID 887—
ReactantWaterHCID 962—
ReactantTriethylamineHCID 8471—
ReactantP,P-Diphenylphosphinic azideHCID 199401—
ReactantHCID 59837328HCID 59837328—
SolventBenzeneHCID 241—
ProductHCID 23078198HCID 23078198—

Reaction Steps

The compound of Example 156 (2.38 g) was dissolved in benzene (20 mL). To this solution, triethylamine (0.711 mL) and DPPA (1.10 mL) were added and the mixture was stirred at room temperature for 10 min, was refluxed, and was further stirred for 1 hour and 30 min. Methanol (3.76 mL) was added over a 30 minute-time period and the mixture was stirred overnight. Subsequently, the reaction mixture was diluted with water and was extracted with ethyl acetate. The ethyl acetate layer was washed with a saturated aqueous solution of sodium chloride, and was then dried over anhydrous magnesium sulfate and was concentrated. The residue was purified on a silica gel column chromatography (hexane:ethyl acetate=20:1 shifted to 5:1) to give the desired product as a yellow oil (2.04 g).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07763752B2
Source datasetuspto-grants-2010_07
ORD IDord-9ba2ff802c714da1ab56cdb1b296a577
Source noteuspto-grants-2010_07