참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Ethyl trifluoroacetate | HCID 9794 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 반응물 | 1-[4-(1H-pyrazol-1-yl)phenyl]ethan-1-one | HCID 12238134 | — |
| 용매 | Ethyl tert-butyl ether | HCID 12512 | — |
| 생성물 | 4,4,4-Trifluoro-1-(4-pyrazol-1-yl-phenyl)-butane-1,3-dione | HCID 68630937 | 63.4% |
반응 단계
A 5.4 N solution of sodium methoxide in methanol (3.0 mL, 16.2 mmol) was added drop wise over 10 min to a solution of ethyl trifluoro-acetate (1.81 mL, 15.2 mmol) in 2-ethoxy-2-methyl-propane (20 mL) at 20° C. followed by the addition of a suspension of 1-(4-pyrazol-1-yl-phenyl)-ethanone (2.57 g, 13.8 mmol) in 2-ethoxy-2-methyl-propane (10 mL). The reaction mixture was stirred for 22 h at 20° C. and then poured onto ice-water (50 mL). The mixture was extracted with ethyl acetate and the organic layer was washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The remaining solid was recrystallized from ethyl acetate/heptane to give the title compound (2.47 g, 63%) as off-white solid. Mp 96° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08962834B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_02 |
|---|
| ORD ID | ord-35d4d44f7e334382a8d9b1f824d5df5c |
|---|
| 출처 메모 | uspto-grants-2015_02 |
|---|