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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 70248Generated: October 25, 2026

Methanol → HCID 178502068, compound

https://huagongshe.com/reaction/70248

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethanolHCID 887—
ReactantAzidotrimethylsilaneHCID 78378—
Reactantmethyl N-[(2-chloro-5-ethynylphenyl)methyl]carbamateHCID 86641518—
CatalystCopper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)HCID 24350—
SolventDimethylformamideHCID 6228—
ProductHCID 178502068HCID 178502068—

Reaction Conditions

Temperature100 °C

Reaction Steps

To a solution of methyl N-[(2-chloro-5-ethynylphenyl)methyl]carbamate (i.e. the product of Step D) (0.43 g, 1.92 mmol) in N,N-dimethylformamide (3.9 mL) and methanol (0.4 mL) was added trimethylsilyl azide (0.38 mL, 2.89 mmol) and copper(I) iodide (0.019 g, 0.1 mmol). The reaction mixture was heated in a CEM Discover microwave apparatus at 100° C. for 8 h and then allowed to cool to room temperature. The reaction mixture was partitioned between ethyl acetate and aqueous sodium chloride, the layers were separated and the aqueous layer was extracted with ethyl acetate (2×). The combined organic layers were washed with water (3×), dried over magnesium sulfate, filtered and concentrated under reduced pressure to provide the title compound, a compound of the present invention, as a brown solid (0.30 g).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08822521B2
Source datasetuspto-grants-2014_09
ORD IDord-35a6f0c7e97740369673e373933633cd
Source noteuspto-grants-2014_09