Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- → 1-(3',4'-Dimethoxyphenyl)-7-(4'-chlorophenyl)-2-nitro-5-heptanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- | HCID 10036050 | — |
| 반응물 | 5-Iodo-1-(4'-chlorophenyl)-3-pentanone | HCID 20164190 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(3',4'-Dimethoxyphenyl)-7-(4'-chlorophenyl)-2-nitro-5-heptanone | HCID 20164188 | 69.6% |
반응 단계
To a solution of 48.5 g (0.23 mole) of 2-(3,4-dimethoxyphenyl)-1-nitroethane in 400 ml of dry tetrahydrofuran was added 96.0 g (0.23 mole) of 40% Triton B. The solution was stirred at room temperature for 10 min. 70.3 g (0.23 mole) of 5-iodo-1-(4'-chlorophenyl)-3-pentanone in a minimum amount of dry tetrahydrofuran was added dropwise. The mixture was heated at 50° C. for 3 hrs., then allowed to stir at room temperature overnight. Solvent was removed in vacuo and the residue taken up in ether and extracted twice with water. The organic layer was dried over anh MgSO4, filtered and concentrated at reduced pressure. The crude concentrate was passed through HPLC to give 65 g of purified material.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04701461 |
| 출처 데이터셋 | uspto-grants-1987_10 |
| ORD ID | ord-40aee1bb3ed343f29a6b74e7cbb84420 |
| 출처 메모 | uspto-grants-1987_10 |