Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
tert-Butyl methyl ether → 2-Methyl-5-[4,4,4-trifluoro-3-hydroxy-3-(3,4,5-trichloro-phenyl)-butyryl]-furan-3-carboxylic acid methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | tert-Butyl methyl ether | HCID 15413 | — |
| 반응물 | Lithium hydride | HCID 62714 | — |
| 반응물 | Methyl 5-acetyl-2-methylfuran-3-carboxylate | HCID 10866962 | — |
| 반응물 | 2,2,2-Trifluoro-1-(3,4,5-trichlorophenyl)ethan-1-one | HCID 58077594 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Methyl-5-[4,4,4-trifluoro-3-hydroxy-3-(3,4,5-trichloro-phenyl)-butyryl]-furan-3-carboxylic acid methyl ester | HCID 86706650 | 123.5% |
반응 단계
LiH (1.76 g) is added to a solution of 2,2,2-trifluoro-1-(3,4,5-trichloro-phenyl)-ethanone (35.33 g) and 5-acetyl-2-methyl-furan-3-carboxylic acid methyl ester (20 g) in THF (300 ml). After 1 hour 30 at 60° C. MTBE is added (450 ml) and the reaction mixture is poured onto water (750 ml) at 0° C. The organic phase is washed with water and a saturated aqueous solution of NaCl dried over MgSO4 and concentrated in vacuo to yield 62.3 g of 2-methyl-5-[4,4,4-trifluoro-3-hydroxy-3-(3,4,5-trichloro-phenyl)-butyryl]-furan-3-carboxylic acid methyl ester. The crude product is used without further purification. MS (HPLC/MS): 459 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822466B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-902876f080bc48ad8e0deb56ed5f2e12 |
| 출처 메모 | uspto-grants-2014_09 |