Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,4,6-Trimethylpyridine → (4R)-N-[(1S)-1-Methyl-2-nitroxyethyl]-2-oxothiazolidin-4-yl-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| 반응물 | Nitronium tetrafluoroborate | HCID 11073463 | — |
| 반응물 | (4R)-N-[(1S)-1-Methyl-2-hydroxyethyl]-2-oxothiazolidin-4-yl-carboxamide | HCID 21309140 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | (4R)-N-[(1S)-1-Methyl-2-nitroxyethyl]-2-oxothiazolidin-4-yl-carboxamide | HCID 9816362 | 29.2% |
반응 단계
In 10 ml of dry acetonitrile were dissolved 478 mg of nitronium tetrafluoroboron (85% content), 0.43 ml of 2,4,6-collidine was added thereto with stirring under ice-cooling, and the mixture was stirred under ice-cooling for 30 minutes. To the resulting mixture were added 500 mg of (4R)-N-[(1S)-1-methyl-2-hydroxyethyl]-2-oxothiazolidin-4-yl-carboxamide, and the mixture was stirred at room temperature for 1 hour and 45 minutes. Then, the solvent was distilled off under reduced pressure and the thus obtained residue was purified by silica gel column chromatography employing cyclohexane-ethyl acetate (3:7) as an eluent to obtain 178 mg of the desired compound as colorless crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05891898 |
| 출처 데이터셋 | uspto-grants-1999_04 |
| ORD ID | ord-e09145e95582489a842ab3d05043dfe5 |
| 출처 메모 | uspto-grants-1999_04 |