Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 6-[2-(5-Bromopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 5-Bromo-2-chloropyrimidine | HCID 606665 | — |
| 반응물 | 2-{6-Amino-5-(4-methylphenyl)-pyrimidin-4-yloxy}ethanol | HCID 11118297 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-[2-(5-Bromopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-amine | HCID 11729102 | 91.1% |
반응 단계
To a solution of 2-{6-amino-5-(4-methylphenyl)pyrimidin-4-yloxy}-ethanol (7.54 g) in tetrahydrofuran (150 ml) is added sodium hydride (60% dispersion-type, 1.47 g), and thereto is added 5-bromo-2-chloropyrimidine (7.73 g), and the mixture is stirred at room temperature overnight. To the reaction solution is added saturated aqueous ammonium chloride solution, and the mixture is evaporated to remove the solvent. The precipitated crystals are collected by filtration, washed and dried. The crude crystals are purified by silica gel column chromatography (solvent; chloroform/methanol=100:1~80:1), and recrystallized from tetrahydrofuran/diethyl ether to give 6-[2-(5-bromopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-amine (11.27 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05728706 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-a7b7ef5f674140eda2b87b65e3637f7d |
| 출처 메모 | uspto-grants-1998_03 |