Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → 3,5-Dichloro-4-(2,2,2-trifluoroethoxy)aniline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Stannous Chloride | HCID 24479 | — |
| 반응물 | 1,3-Dichloro-5-nitro-2-(2,2,2-trifluoroethoxy)benzene | HCID 13852227 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 3,5-Dichloro-4-(2,2,2-trifluoroethoxy)aniline | HCID 13852146 | 94% |
반응 단계
To a solution of 1,3-dichloro-5-nitro-2-(2,2,2-trifluoroethoxy)benzene (1.90 g, 6.55 mmol) in MeOH (20 mL) and 12 N HCl (20 mL) at rt, SnCl2 (3.72 g, 19.66 mmol) was slowly added to it and then the reaction mixture was stirred overnight at rt. To the reaction mixture was slowly added 3N NaOH to pH=10 and then extracted with EA. The combined organic layers were washed with brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure. The residue was purified by column chromatography over silica gel eluted with PE:EA (6:1) to provide 3,5-dichloro-4-(2,2,2-trifluoroethoxy)aniline (1.60 g, yield 94%) as pale yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08853186B2 |
| 출처 데이터셋 | uspto-grants-2014_10 |
| ORD ID | ord-ae1e0c4f0cb74bbb84f8d051cd35e0bd |
| 출처 메모 | uspto-grants-2014_10 |