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Triethylamine → HCID 178418686、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | HCID 178418587 | HCID 178418587 | — |
| 触媒 | Palladium Chloride | HCID 24290 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 178418686 | HCID 178418686 | — |
反応手順
A mixture of 2.0 g of 3-iodo-4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]pyrimidine, 1.2 g. of trimethylsilylacetylene, 0.1 g of palladium chloride, 0.23 g of triphenylphosphine, 0.06 g of cuprous iodide, and 2.6 g of triethylamine in 100 mL of acetonitrile is heated in a sealed tube for 1.5 hours at 50° C. and then at reflux for 3 hours. The solvent is removed under reduced pressure and the residue triturated with 1:1 ethyl acetate:hexanes and filtered. The solid thus collected is dissolved in methylene chloride and this solution is passed through a pad of silica gel eluting with 1% methanol on methylene chloride. The eluate is concentrated to yield 3-trimethylsilylethynyl-4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]pyrimidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05248775 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-60b4f2f7c4364d6ea701f73a82cf4b0f |
| 出典メモ | uspto-grants-1993_09 |