참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Trimethylsilylacetylene | HCID 66111 | — |
| 반응물 | 5-Bromo-2-hydroxy-4-methyl-3-nitropyridine | HCID 21706517 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 5-Trimethylsilylethynyl-4-methyl-3-nitro-2-pyridone | HCID 21706491 | 96.4% |
반응 단계
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%)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06054470 |
|---|
| 출처 데이터셋 | uspto-grants-2000_04 |
|---|
| ORD ID | ord-c9f1bf0a91384fa1b2adf3e397b54aee |
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| 출처 메모 | uspto-grants-2000_04 |
|---|
