Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-(2',4'-Difluoro(1,1'-biphenyl)-4-yl)ethan-1-one → 3-(2',4'-Difluoro-4-biphenylyl)-2-butenoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-(2',4'-Difluoro(1,1'-biphenyl)-4-yl)ethan-1-one | HCID 104542 | — |
| 반응물 | Lithium diisopropylamide | HCID 2724682 | — |
| 반응물 | Dibenzylphosphonoacetic acid | HCID 5104966 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-(2',4'-Difluoro-4-biphenylyl)-2-butenoic acid | HCID 54010068 | — |
반응 단계
A solution of 21.4 g. of lithium diisopropylamide in 200 ml. of THF is added to a stirred solution of 32 g. of α-dibenzylphosphonoacetic acid (carboxymethylphosphonic acid dibenzyl ester) in 300 ml. of THF at -80°. Then a solution of 23.2 g. of 4-acetyl-2',4'-difluorobiphenyl in 250 ml. of THF is asdded. The mixture is stirred for 12 hours more, during which it is allowed to come to room temperature. The product Z--C(CH3)(OLi)--CH[P=O (OCH2C6H5)2 ]COOLi (Z is 2',4'-difluoro-4-biphenylyl), which is formed, is hydrolyzed with dilute acetic acid/ice. The customary work up gives 3-(2',4'-difluoro-4-biphenylyl)-2-butenoic acid, m.p. 193°-195°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04151302 |
| 출처 데이터셋 | uspto-grants-1979_04 |
| ORD ID | ord-800b6243d23c49439f3b8423d4af8ae4 |
| 출처 메모 | uspto-grants-1979_04 |