Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetone → 1-Ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetone | HCID 180 | — |
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | 7-(3-Chloropropoxy)-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione | HCID 68673253 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-Ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione | HCID 68672792 | 99.7% |
반응 단계
7-(3-Chloropropoxy)-1-ethyl-3,3,5-trimethyl-1,5-dihydro-benzo[b][1,4]diazepine-2,4-dione (2.18 g) and sodium iodide (4.8 g) were added to acetone (50 ml), and heated under reflux for 8.5 hours. The reaction mixture was cooled to room temperature, water was added, and extraction with ethyl acetate was performed. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1). The purified product was concentrated under reduced pressure to give the title compound (2.76 g) as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822453B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-59dd04d6f65c49a195f1d8fc186758b4 |
| 출처 메모 | uspto-grants-2014_09 |