Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Ethyl 1,2,3,4-tetrahydro-3-methyl-1-(2-methylpropyl)-2,4-dioxo-6-(4-quinolinylmethyl)thieno[2,3-d]pyrimidine-5-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Trifluoroacetic anhydride | HCID 9845 | — |
| 반응물 | Ethyl 1,2,3,4-tetrahydro-6-(hydroxy-4-quinolinylmethyl)-3-methyl-1-(2-methylpropyl)-2,4-dioxothieno[2,3-d]pyrimidine-5-carboxylate | HCID 5282569 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Ethyl 1,2,3,4-tetrahydro-3-methyl-1-(2-methylpropyl)-2,4-dioxo-6-(4-quinolinylmethyl)thieno[2,3-d]pyrimidine-5-carboxylate | HCID 5282570 | — |
반응 단계
Trifluoroacetic anhydride (3.33 ml) was added to a solution of the product of step b) (7.34 g) and triethylamine (6.56 ml) in anhydrous THF (150 ml) at room temperature under nitrogen and the mixture stirred for 15 min. 10% palladium on charcoal (500 mg) was added and the mixture hydrogenated at 1 bar for 20 h. It was filtered through Celite, washing with saturated sodium bicarbonate solution (150 ml) then ethyl acetate (300 ml). The organic material was extracted into ethyl acetate (150 ml), the combined extracts were dried over magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography, eluting with 1:1 ethyl acetate/i-hexane, to give the sub-title compound as a solid (5.90 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07361660B2 |
| 출처 데이터셋 | uspto-grants-2008_04 |
| ORD ID | ord-24dd1a48d42240608b7f018ebdea3c53 |
| 출처 메모 | uspto-grants-2008_04 |