Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Hydroxide → 4,6-Bis(1,1-dimethylethyl)-5-hydroxy 2-methylpyrimidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | 1-[4-(1,1-Dimethylethyl)-2-methyl-5-oxazolyl]-2,2-dimethyl-1-propanone | HCID 18925378 | — |
| 생성물 | 4,6-Bis(1,1-dimethylethyl)-5-hydroxy 2-methylpyrimidine | HCID 9877866 | 75% |
반응 단계
A mixture of 1-[4-(1,1-dimethylethyl)-2 methyl-5-oxazolyl]-2,2-dimethyl-1 propanone (8.5 g, 38 mmol) and concentrated ammonium hydroxide (100 mL) is heated at 180° C. for 36 hours in a steel bomb. The reaction mixture is cooled and the excess ammonia is evaporated on the rotovap. The pH of the resulting mixture is adjusted to pH 6 with concentrated HCl with ice bath cooling. The product is extracted into ether (3×250 mL) and the organic layer is dried (MgSO4) and evaporated. The residue is purified by flash chromatography (silica, 7% EtOAc/hexane) to give pure 4,6-bis(1,1-dimethylethyl)-5-hydroxy-2-methylpyrimidine (6.35 g, 75%) as a partial hydrate; mp 62°-65° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05248682 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-c60e5ad8c697434fa67dd662437ae58d |
| 출처 메모 | uspto-grants-1993_09 |