戻る
化工社化工社 化学情報印刷レポート · 研究参考用
HRID 70248作成日:2026年10月25日

Methanol → HCID 178502068、化合物

https://huagongshe.com/reaction/70248

反応式

関与物質

役割名称HCID仕込み量
反応物MethanolHCID 887—
反応物AzidotrimethylsilaneHCID 78378—
反応物methyl N-[(2-chloro-5-ethynylphenyl)methyl]carbamateHCID 86641518—
触媒Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)HCID 24350—
溶媒DimethylformamideHCID 6228—
生成物HCID 178502068HCID 178502068—

反応条件

温度100 °C

反応手順

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).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08822521B2
出典データセットuspto-grants-2014_09
ORD IDord-35a6f0c7e97740369673e373933633cd
出典メモuspto-grants-2014_09