Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Bicarbonate → 4-(6-Bromo-4-methyl-3-oxo-3,4-dihydro-pyrazin-2-ylamino)-benzaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Tempo | HCID 2724126 | — |
| 반응물 | 5-Bromo-3-(4-hydroxymethyl-phenylamino)-1-methyl-1H-pyrazin-2-one | HCID 58728996 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-(6-Bromo-4-methyl-3-oxo-3,4-dihydro-pyrazin-2-ylamino)-benzaldehyde | HCID 58728909 | — |
반응 단계
Compound (2) (3.1 g; 10 mmol) was dissolved in 150 mL CH2Cl2 at rt under N2. Solid 12 (5.1 g; 20 mmol) was added portion-wise to the stirring reaction, followed by catalytic 2,2,6,6-tetramethyl-1-piperdinyloxy, free radical (TEMPO; 0.23 g; 1.50 mmol). Saturated sodium bicarbonate solution was then added (20 mL) and the reaction allowed to stir overnight at rt under N2. The resulting light orange solid was filtered off and washed repeatedly with CH2Cl2 and diethyl ether until the extractions ran clear and colorless. After drying, 4-(6-bromo-4-methyl-3-oxo-3,4-dihydro-pyrazin-2-ylamino)-benzaldehyde (3) was obtained in nearly quantitative yields (3.1 g) and was carried directly on to the next reaction. MS 308.01 & 310.01 (M+H)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07947835B2 |
| 출처 데이터셋 | uspto-grants-2011_05 |
| ORD ID | ord-d7d45fec2b7b410bb267653d07ccdd85 |
| 출처 메모 | uspto-grants-2011_05 |