関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | 5-Bromo-2-hydroxy-4-methyl-3-nitropyridine | HCID 21706517 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 5-Trimethylsilylethynyl-4-methyl-3-nitro-2-pyridone | HCID 21706491 | 96.4% |
反応手順
A mixture of 5-bromo-4-methyl-3-nitro-2-pyridone (1.0 g, 2.8 mmol), trimethylsilylacetylene (1.2 mL, 8.5 mmol), bis(triphenylphosphine)Pd(II) chloride (0.100 g) and cuprous iodide (0.025 g) in DMF (4 mL) and triethylamine (2 mL) was heated at 90 ° C. in a sealed tube for 7 hours. Ethyl acetate was added, and the mixture was washed with water, dried, filtered and evaporated. Chromatography of the residue over silica gel (40% ethyl acetate/hexane) gave 5-trimethylsilylethynyl-4-methyl-3-nitro-2-pyridone (1.0 g, 2.7 mmol, 96%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06054470 |
|---|
| 出典データセット | uspto-grants-2000_04 |
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| ORD ID | ord-c9f1bf0a91384fa1b2adf3e397b54aee |
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| 出典メモ | uspto-grants-2000_04 |
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