Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Formamidine acetate → tert-Butyl 7,8-dihydropyrido[4,3-d]pyrimidine-6(5H)-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Formamidine acetate | HCID 160693 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 반응물 | tert-butyl 3-[(dimethylamino)methylene]-4-oxotetrahydro-1(2H)-pyridinecarboxylate | HCID 53395404 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | tert-Butyl 7,8-dihydropyrido[4,3-d]pyrimidine-6(5H)-carboxylate | HCID 22707088 | — |
반응 단계
Formamidine acetate (472 mg, 4.52 mmol) in 15.0 mL of absolute ethanol was treated with sodium ethoxide (21 wt % solution in ethanol; 1.7 mL). After 30 min, a solution of the product from Step A above (1.15 g) in 8 mL of absolute ethanol was added, and the mixture was warmed at reflux for 18 h. The dark solution was cooled to room temperature and concentrated under reduced pressure, and the residue was partitioned between ethyl acetate and water. The organic layer was separated, washed with brine, dried over magnesium sulfate and concentrated to an orange oil. Purification by flash chromatography (silica gel; 2% methanol/dichloromethane as eluant) afforded the title compound as a light yellow gum.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07388019B2 |
| 출처 데이터셋 | uspto-grants-2008_06 |
| ORD ID | ord-66ae1acf66014a01b5eaced42a3466dd |
| 출처 메모 | uspto-grants-2008_06 |