Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Anhydride → N-(6-chloro-3-nitropyridin-2-yl)acetamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 6-Chloro-3-nitropyridin-2-ylamine | HCID 2724035 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | N-(6-chloro-3-nitropyridin-2-yl)acetamide | HCID 2783822 | 8.2% |
반응 단계
To a suspension of sodium hydride (120 mg, 5 mmole) in tetrahydrofuran(10 ml), a solution of 2-amino-3-nitro-6-chloropyridine (870 mg, 5 mmole) in 20 ml of tetrahydrofuran (20 ml) was added. The reaction mixture was stirred at room temperature for 30 min. A solution of acetic anhydride (377 μl, 6 mmole) in tetrahydrofuran (10 ml) was added and stirred at room temperature overnight. The reaction mixture was quenched with water and concentrated under reduced pressure. The crude product was dissolved in dichloromethane and washed with brine. The organic layer was dried with sodium sulfate and then concentrated under vacuo. The crude was purified by flash chromatography, eluting 78% hexane: 22% ethyl acetate to give a yellow product (88 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07425557B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-ff23ce087624488a9ff18ee824f2f51f |
| 출처 메모 | uspto-grants-2008_09 |