Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → HCID 178503295, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Methyl 2-cyano-3,3-bis(methylsulfanyl)prop-2-enoate | HCID 319957 | — |
| 반응물 | 2-Cyanoethanethioamide | HCID 1416277 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | HCID 178503295 | HCID 178503295 | — |
반응 단계
2-cyano-3,3-bis-methylsulfanyl-acrylic acid methyl ester Compound 1a (25.0 g, 123 mmol) was combined with 97% 2-cyano-thioacetamide (12.7 g, 123 mmol) and K2CO3 (51.0 g, 369 mmol) in DMSO (300 mL) at room temperature. The reaction was stirred for 18 hrs. The cooled reaction mixture (0° C.) was slowly acidified with 1N HCl. The resultant yellow precipitate was collected by filtration and sequentially washed with 1N HCl, water, MeOH and hexane to give 6-hydroxy-4-methylsulfanyl-2-thioxo-1,2-dihydro-pyridine-3,5-dicarbonitrile Compound 1b (24.7 g, 90% yield). 1H NMR (DMSOd6) δ 2.66 (s, 3H). 13C NMR (DMSOd6) δ 118.1 (CN), 117.3 (CN), 17.4 (SMe). MS 222 (M−).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07427625B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-4e9eb525ff6140618b62125cd778740a |
| 출처 메모 | uspto-grants-2008_09 |