Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cyanoacetamide → 1,2-Dihydro-6-methyl-2-oxo-5-phenyl-3-pyridinecarbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cyanoacetamide | HCID 7898 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 3-Buten-2-one, 4-(dimethylamino)-3-phenyl- | HCID 1488369 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1,2-Dihydro-6-methyl-2-oxo-5-phenyl-3-pyridinecarbonitrile | HCID 20231 | — |
반응 단계
A mixture of 4-dimethylamino-3-phenyl-3-butene-2-one (14.1 grams) and cyanoacetamide (5.9 grams) in 100 ml methanol was added to sodium methoxide (7.9 grams) in 100 ml methanol. The mixture was refluxed for 18 hours and then the crude reaction was stripped and the residue dissolved in a small amount of hot water. Acidification to pH 6-7 gave a gum-like solid which was collected by filtration. Further acidification to a lower pH gave only an oil. Trituration of the gum with ethyl acetate and chilling resulted in an off-white solid which was identified by NMR as the desired product, yield 2.8 grams, m.p. 280°-290° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04405552 |
| 출처 데이터셋 | uspto-grants-1983_09 |
| ORD ID | ord-ac9ef9b7538d471e8226a7b9c029c0e4 |
| 출처 메모 | uspto-grants-1983_09 |