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Tetrahydrofuran → 5-Bromo-6-[2-tri(propan-2-yl)silylethynyl]pyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (Triisopropylsilyl)acetylene | HCID 2734682 | — |
| 反応物 | 5,6-Dibromopyridin-2-amine | HCID 13692781 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-Bromo-6-[2-tri(propan-2-yl)silylethynyl]pyridin-2-amine | HCID 86694366 | — |
反応手順
A mixture of 5,6-dibromopyridin-2-amine (60 g, 233 mmol), ethynyl-tri(propan-2-yl)silane (64 ml, 285 mmol), copper(I) iodide (1.5 g, 7.88 mmol), Dichlorobis(triphenylphosphine)-palladium(II) (4.0 g, 5.48 mmol) and triethylamine (80 ml, 577 mmol) is stirred under argon atmosphere in ACN (200 ml) with THF (100 ml) for 2 h at 50° C. The mixture is concentrated in vacuo and the product purified by NP chromatography. Yield: 76 g (92%). HPLC-MS: M+H=353/355; tR=1.79 min (*Method—1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08859541B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-03725f62953a43cb9ebe0a17b9fc9316 |
| 出典メモ | uspto-grants-2014_10 |