Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl 4,4,4-trifluoroacetoacetate → 4-Trifluoromethyl-8-propyl-7-hydroxycoumarin
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl 4,4,4-trifluoroacetoacetate | HCID 67793 | — |
| 반응물 | 1,3-Benzenediol, propyl- | HCID 262060 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-Trifluoromethyl-8-propyl-7-hydroxycoumarin | HCID 53701430 | 77% |
반응 단계
2-propylbenzene-1,3-diol (J. Med. Chem., 38, pp 4411-4432, 1995) (3.65 g, 24.0 mmol), zinc chloride (3.60 g, 26.4 mmol), and ethyl 4,4,4-trifluoroacetoacetate (4.86 g, 26.4 mmol) were stirred overnight at 110° C. The reaction solution was added with water and extracted with ethyl acetate. Subsequently, the organic layer was washed with saturated saline, dried using anhydrous sodium sulfate, and concentrated under vacuum. The obtained residue was purified using silica-gel chromatography (chloroform) and then recrystallized with chloroform, and 5.01 g of the title compound (yield 77%) was obtained as pale-brown crystalline powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07919509B2 |
| 출처 데이터셋 | uspto-grants-2011_04 |
| ORD ID | ord-f96cc53798e64e878eaa111501b118ce |
| 출처 메모 | uspto-grants-2011_04 |