Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 1,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Ethyl trifluoroacetate | HCID 9794 | — |
| 반응물 | 1-(4-(Methylthio)phenyl)ethan-1-one | HCID 74501 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 생성물 | 1,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]- | HCID 10730170 | 71% |
반응 단계
To a solution of ethyl trifluoroacetate (7.95 ml, 1.1 eq) in MTBE (125 ml) was added dropwise 25% sodium methoxide in methanol (16 ml, 1.2 eq). 4-Methylthioacetophenone (Aldrich, 10 g, 0.06 mol) was added portionwise and the mixture stirred at ambient temperature overnight. 2N Hydrochloric acid (40 ml) was added cautiously and the organic phase separated, washed with brine and dried (Na2SO4) to give an orange solid. The orange solid was recrystallised from hot isopropanol to give the title compound as a yellow crystalline solid (11.25 g, 71%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07084148B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-697eb1beb35a4059a73112f3071f16a1 |
| 출처 메모 | uspto-grants-2006_08 |