Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
5-Chlorosalicylic Acid → Imd-0354
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 5-Chlorosalicylic Acid | HCID 9447 | — |
| 반응물 | Benzenamine, 3,5-bis(trifluoromethyl)- | HCID 9480 | — |
| 반응물 | Phosphorus trichloride | HCID 24387 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Imd-0354 | HCID 5081913 | 57% |
반응 단계
To 30 ml of toluene were added 5-chlorosalicylic acid (862 mg, 5 mmol), 3,5-bis(trifluoromethyl)aniline (1.37 g, 6 mmol), and phosphoroustrichloride (755 mg, 5.5 mmol) in the presence of argon gas, followed by stirring for 6 hours through heat-reflux. Sodium hydrogen carbonate was added to the mixture to adjust pH to 7, followed by concentration under reduced pressure. The mixture was dissolved in 60 ml of ethylacetate, which was washed with water (40 ml×2). The organic layer was concentrated under reduced pressure, followed by column chromatography to give 1.09 g of the target compound (yield: 57%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09266872B2 |
| 출처 데이터셋 | uspto-grants-2016_02 |
| ORD ID | ord-345a9614066d4029ad26aef33ddc90bf |
| 출처 메모 | uspto-grants-2016_02 |