Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 5-Bromo-6-[2-(5-methylthiopyrimidin-2-yloxy)ethoxy]pyrimidine-4-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2-(6-Amino-5-bromopyrimidin-4-yloxy)ethanol | HCID 18931106 | — |
| 반응물 | 2-Chloro-5-(methylthio)pyrimidine | HCID 21979532 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-Bromo-6-[2-(5-methylthiopyrimidin-2-yloxy)ethoxy]pyrimidine-4-amine | HCID 19689525 | 53.6% |
반응 단계
To a solution of 2-(6-amino-5-bromopyrimidin-4-yloxy)ethanol (611 mg) in dimethylformamide (20 ml) is added sodium hydride (60% dispersion-type, 125 mg), and the mixture is stirred for 20 minutes. To the mixture is added 2-chloro-5-methylthiopyrimidine (461 mg), and the mixture is stirred at room temperature for three hours. To the mixture is added ice-water, and the mixture is extracted with ethyl acetate. The ethyl acetate layer is washed, dried, and evaporated to remove the solvent. The residue is purified by silica get column chromatography (solvent; chloroform/methanol=20:1), and crystallized from ethyl acetate/diisopropyl ether to give 5-bromo-6-[2-(5-methythiopyrimidin-2-yloxy)ethoxy]pyrimidine-4-amine (501 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05728706 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-4bd91debc1224985b59b17dd05823067 |
| 출처 메모 | uspto-grants-1998_03 |