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Trimethylsilylacetylene → HCID 14373291、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | 6-Bromo-3,4-dihydroquinolin-2(1H)-one | HCID 14373281 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | HCID 14373291 | HCID 14373291 | — |
反応手順
A mixture of 8.0 g of 6-bromo-3,4-dihydrocarbostyril, 6.95 g of trimethylsilylacetylene, 460 mg of bis(triphenylphosphine)palladium dichloride and 62 mg of cuprous iodide in 53 ml of pyridine and 11 ml of triethylamine was refluxed for 3 days. The solvent was removed under reduced pressure, 50 ml of methanol added along with 300 mg of potassium carbonate, and the mixture stirred under nitrogen for 18 hours. The solvent was removed under reduced pressure and the residue chromatographed on silica gel, eluting with 3% methanol in methylene chloride, giving a product of 6-ethynyl-3,4-dihydrocarbostyril, m.p. 182°-184° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04792561 |
| 出典データセット | uspto-grants-1988_12 |
| ORD ID | ord-5620a142c0124c1082c104c5c4d5667c |
| 出典メモ | uspto-grants-1988_12 |