Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 4,7-Dichloro-6-nitroquinazoline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 7-Chloro-6-nitroquinazolin-4(1H)-one | HCID 135687504 | — |
| 용매 | Thionyl Chloride | HCID 24386 | — |
| 생성물 | 4,7-Dichloro-6-nitroquinazoline | HCID 10490455 | 81% |
반응 단계
A mixture of 7-chloro-6-nitro-3,4-dihydroquinazolin-4-one (40 g, 0.18 mol), (J. Org. Chem. 1975, 40, 356), phosphorus oxychloride (50 ml) and DMF (1 ml) in thionyl chloride (300 ml) was heated at reflux for 4 hours. The reaction mixture was allowed to cool and the volatiles removed by evaporation and by azeotroping with toluene. The residue was basified with aqueous sodium hydrogen carbonate solution and extracted with methylene chloride (4×100 ml). The extracts were combined, washed with brine and filtered through phase separating paper. The solvent was removed by evaporation and the residue triturated with ether/isohexane to give 4,7-dichloro-6-nitroquinazoline (35.2 g, 81%) as a pale yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06673803B2 |
| 출처 데이터셋 | uspto-grants-2004_01 |
| ORD ID | ord-9337bab50e5f4d94846c3b598158b530 |
| 출처 메모 | uspto-grants-2004_01 |