Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Chloro-5-nitropyrimidine → 2-[(3,3-Dimethyl-2,3-dihydro-1-benzofuran-4-yl)oxy]-5-nitropyrimidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Chloro-5-nitropyrimidine | HCID 82544 | — |
| 반응물 | 3,3-Dimethyl-2,3-dihydro-1-benzofuran-4-ol | HCID 57411299 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-[(3,3-Dimethyl-2,3-dihydro-1-benzofuran-4-yl)oxy]-5-nitropyrimidine | HCID 67958694 | 99.2% |
반응 단계
To a solution of 3,3-dimethyl-2,3-dihydro-1-benzofuran-4-ol (Intermediate 50, 724 mg) in dry N,N-Dimethylformamide (40 mL) potassium carbonate and 2-chloro-5-nitropyrimidine (774 mg, 4.85 mmol) were added. The reaction mixture was stirred at room temperature overnight. The reaction was quenched with water (40 ml) and extracted with ethyl acetate (3×40 ml). The combined organic layers were washed with brine (2×50 ml), separated, dried over sodium sulphate, filtered and evaporated. The residue was purified by flash chromatography on silica gel using a column SNAP 50 g and cyclohexane/ethyl acetate as eluents from 100/0 to 70/30 to afford the title compound (1.257 g) as a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09346790B2 |
| 출처 데이터셋 | uspto-grants-2016_05 |
| ORD ID | ord-91d41efbafce4aa18e70f89123c515be |
| 출처 메모 | uspto-grants-2016_05 |