Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,3-Dimethyl-2-imidazolidinone → 2-Chloro-6-nitro-4-pentylaminoquinazoline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,3-Dimethyl-2-imidazolidinone | HCID 6661 | — |
| 반응물 | Propylamine | HCID 7852 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 6-Nitro-2,4(1H,3H)-quinazolinedione | HCID 816982 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Chloro-6-nitro-4-pentylaminoquinazoline | HCID 18326391 | 70.1% |
반응 단계
To 400 mg (1.93 mmol) of 6-nitroquinazoline-2,4 (1H,3H)-dione were added 1 ml of 1,3-dimethyl-2-imidazolidinone and 6.58 g (42.91 mmol) of phosphorus oxychloride, and the resulting mixture was subjected to heating under reflux for 3 hours. After phosphorus oxychloride was removed in vacuo, the mixture was dissolved in 4 ml of acetonitrile, followed by addition of 5.60 ml (48.25 mmol) of propylamine and stirring under ice cooling for 30 minutes. To the reaction solution was added water, followed by extraction with ethyl acetate, washing with brine and drying over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by a silica gel column to give 342 mg (yield: 70.1%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06339089B2 |
| 출처 데이터셋 | uspto-grants-2002_01 |
| ORD ID | ord-0462c276a4144fca94d466f1c3282fd4 |
| 출처 메모 | uspto-grants-2002_01 |