Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Chloride → 2-Chloro-5-(2,3-difluorobenzoyl)pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 1-Bromo-2,3-difluorobenzene | HCID 2733260 | — |
| 반응물 | 6-Chloro-N-methoxy-N-methylnicotinamide | HCID 11435597 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Chloro-5-(2,3-difluorobenzoyl)pyridine | HCID 22626662 | 77% |
반응 단계
To a solution of 1-bromo-2,3-difluorobenzene (0.114 g, 0.746 mmol) in 3 ml of dry THF was added, at −78° C., n-butyl lithium (1.6 M in hexane, 0.47 ml, 0.749 mmol). The reaction mixture was stirred at this temperature for 1 hour. A solution of 6-chloro-N-methoxy-N-methyl-nicotinamide (0.13 g, 0.68 mmol) in 5 ml of THF was added and the reaction mixture was allowed to warm to RT and stir for 6 hours. Saturated NH4Cl was added and the mixture was extracted with CH2Cl2 (3×10 ml). The organic layers were combined, washed with brine, and dried over NaSO4. The solvents were removed in vacuo and the residue was purified by column chromatography (Hex/AcOEt 9:1) to give 130 mg (77%) of an oily product. IR, NMR.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06358971B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-cb0eaa22d06545359b18611473bc8c02 |
| 출처 메모 | uspto-grants-2002_03 |