Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 3-Chloro-5-methoxybenzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 3,5-Dichlorobenzonitrile | HCID 81052 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-Chloro-5-methoxybenzonitrile | HCID 21949921 | 86.5% |
반응 단계
step 1—A 100 ml round bottom flask was charged under a stream of nitrogen with 3,5-dichlorobenzonitrile (R-3a,7.0 g, 40.69 mmol) and anhydrous DMF (75 mL). To the solution was added sodium methoxide (2.26 g, 44.76 mmol) and resulting solution was stirred further at RT for 24 h. When the reaction was complete, aqueous 10% HCl added dropwise to the reaction vessel. The crude mixture was extracted with EtOAc and sequentially washed with aqueous acid, water and brine. The EtOAc extracts were dried (Na2SO4), filtered and the solvent was removed in vacuo to afford a crude solid which was recrystallized from hexane/acetone to afford 5.9 g (86%) of 5-chloro-3-methoxy-benzonitrile.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07906540B2 |
| 출처 데이터셋 | uspto-grants-2011_03 |
| ORD ID | ord-7f8e5d2ac95b4b8ba3b792073f11181f |
| 출처 메모 | uspto-grants-2011_03 |