Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Toluene → Imd-0354
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | 5-Chlorosalicylic Acid | HCID 9447 | — |
| 반응물 | Benzenamine, 3,5-bis(trifluoromethyl)- | HCID 9480 | — |
| 반응물 | Phosphorus trichloride | HCID 24387 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Imd-0354 | HCID 5081913 | 85.5% |
반응 단계
A mixture of 5-chlorosalicylic acid(6.90 g, 40 mmol), 3,5-bis(trifluoromethyl)aniline(9.16 g, 40 mmol), phosphorus trichloride(1.74 mL, 20 mmol) and toluene(80 mL) was refluxed for 3 hours under argon atmosphere. After the reaction mixture was cooled to room temperature, it was diluted with ethyl acetate (240 mL). After the ethyl acetate layer was washed successively with water and brine, dried over anhydrous magnesium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=4:1) to give the title compound (13.12 g, 85.5%) as a light yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07626042B2 |
| 출처 데이터셋 | uspto-grants-2009_12 |
| ORD ID | ord-15e5a58d6dda499799ed9adf297e061d |
| 출처 메모 | uspto-grants-2009_12 |