Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cyanoacetamide → 5-Ethyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cyanoacetamide | HCID 7898 | — |
| 반응물 | 2-Ethyl-3-oxobutanol | HCID 270299 | — |
| 반응물 | Piperidinium acetate | HCID 3014295 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5-Ethyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile | HCID 10241109 | — |
반응 단계
Accordingly to the method described in J. Heterocyclic Chem., 24, 351 (1987), a mixture 2-ethyl-3-oxobutanol, sodium salt (37.5 g, 0.275 mol), cyanoacetamide (25.2 g, 0.30 mol), aqueous piperidinium acetate (22 mL) [prepared from glacial acetic acid (4.2 mL), water (10 mL) and piperidine (7.2 mL)] in water (775 ml) was refluxed for four hours. Glacial acetic acid (30 ml) was added cautiously (much foaming) as the product precipitated. Upon cooling to room temperature, the product was collected by filtration, washed with cold water and air dried to yield 22.3 g (50%), m.p. 237°-240° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05387512 |
| 출처 데이터셋 | uspto-grants-1995_02 |
| ORD ID | ord-3a7b3ceddd7744df9e57264e8f93a1de |
| 출처 메모 | uspto-grants-1995_02 |