Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl p-tolylacetate → 5-(4-Methyl-benzyl)-3-(1-methyl-4-phenyl-butyl)-3,6-dihydro-[1,2,3]triazolo[4,5-d]pyrirnidin-7-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl p-tolylacetate | HCID 90265 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 반응물 | 5-Amino-1-(1-methyl-4-phenyl-butyl)-1H-[1,2,3]triazole-4-carboxamide | HCID 11149992 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 5-(4-Methyl-benzyl)-3-(1-methyl-4-phenyl-butyl)-3,6-dihydro-[1,2,3]triazolo[4,5-d]pyrirnidin-7-one | HCID 135484611 | 57.9% |
반응 단계
1.0 g (3.8 mmol) of 5-amino-1-(1-methyl-4-phenyl-butyl)-1H-[1,2,3]triazole-4-carboxamide are dissolved in a solution of 439 mg of sodium (19 mmol) in 38 ml of ethanol. 2.22 g (14.6 mmol) of methyl 4-methylphenylacetate are added, and the mixture is then refluxed overnight. The solvent is removed under reduced pressure, the residue is taken up with CH2Cl2, the organic phase is extracted twice with 1N HCl and dried over Na2SO4 and the solvent is removed under reduced pressure. Two chromatographic purifications (cyclohexane/ethyl acetate=3:1) give 853 mg (57%) of a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06458796B1 |
| 출처 데이터셋 | uspto-grants-2002_10 |
| ORD ID | ord-1460cf51abcd4fcea40d48200be58237 |
| 출처 메모 | uspto-grants-2002_10 |