Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Toluene → 4-tert-amyl-N-{6-[2-(5-bromopyridin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 6-[2-(5-Bromopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-amine | HCID 11729102 | — |
| 반응물 | 4-(2-Methylbutan-2-yl)benzene-1-sulfonyl chloride | HCID 22281976 | — |
| 촉매 | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| 용매 | Ammonium Chloride | HCID 25517 | — |
| 생성물 | 4-tert-amyl-N-{6-[2-(5-bromopyridin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide | HCID 19689488 | — |
반응 단계
A mixture of 6-[2-(5-bromopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-amine (150 mg), 4-tert-amylbenzenesulfonyl chloride (184 mg), 96% potassium hydroxide (powder, 300 mg), tetrabutylammonium hydrogen sulfate (34 mg) and toluene (10 ml) is stirred at room temperature overnight. The mixture is diluted with saturated aqueous ammonium chloride solution, and extracted with ethyl acetate. The ethyl acetate layer is washed, dried, and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1), and recrystallized from hexane/ethyl acetate to give 4-tert-amyl-N-{6-[2-(5-bromopyridin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide (188 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05589478 |
| 출처 데이터셋 | uspto-grants-1996_12 |
| ORD ID | ord-b065fb797d834479958f8737ac1e6783 |
| 출처 메모 | uspto-grants-1996_12 |