Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Fluoro-2-nitrobenzene → (4-Methyl-pyridin-3-yl)-(2-nitro-phenyl)-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Fluoro-2-nitrobenzene | HCID 73895 | — |
| 반응물 | 3-Amino-4-picoline | HCID 137935 | — |
| 반응물 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | (4-Methyl-pyridin-3-yl)-(2-nitro-phenyl)-amine | HCID 12361028 | 28.32% |
반응 단계
1M LiHMDS solution (9.25 mL, 9.25 mmol) in THF was added drop wise to a cooled solution of 4-Methyl-pyridin-3-ylamine (1 g, 9.25 mmol) in THF (10 mL) at 0° C. under nitrogen atmosphere. The resulting mixture was added drop wise to a solution of 1-fluoro-2-nitro-benzene (0.98 mL, 9.25 mmol) in THF at 0° C. The resulting reaction mass was stirred at room temperature overnight. The reaction was monitored by TLC (50% ethyl acetate in hexane). The reaction mixture was diluted with ethyl acetate and concentrated under reduced pressure. The crude residue was purified by column chromatography on silica gel (50% ethyl acetate in hexane) to afford 600 mg of the product (28.32% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | USRE045173E1 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-9668a2ae2410479d8a21bac1ca13349d |
| 출처 메모 | uspto-grants-2014_09 |