Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 3-(3-Cyano-thiophen-2-yl)-3-oxo-propionic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Lithium Bromide | HCID 82050 | — |
| 반응물 | 2,2-Bis(trimethylsilyl)propanedioate | HCID 22224580 | — |
| 반응물 | 3-Cyanothiophene-2-carbonyl chloride | HCID 22224749 | — |
| 용매 | Isopropenyl acetate | HCID 7916 | — |
| 생성물 | 3-(3-Cyano-thiophen-2-yl)-3-oxo-propionic acid | HCID 22224915 | — |
| 생성물 | 6-(3-Cyano-thiophen-2-yl)-2,2-dimethyl-[1,3]dioxin-4-one | HCID 22224916 | — |
반응 단계
The 3-(3-cyano-thiophen-2-yl)-3-oxo-propionic acid was prepared from 3-cyano-thiophene-2-carbonyl chloride (24.33 g, 140.6 mmol) and bis(trimethylsilyl)malonate (38.0 mL, 147.7 mmol) with Et3N (41 mL, 295.4 mmol) and LiBr (13.5 g, 154.7 mmol) in CH3CN at 0° C. according to general procedure H (method c1). The crude material (24.8 g) was transformed into the title compound by stirring in isopropenyl acetate and conc. H2SO4 according to general procedure J (method a). Obtained as an orange solid (5.6 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07018998B2 |
| 출처 데이터셋 | uspto-grants-2006_03 |
| ORD ID | ord-32d8d277e8c847da9ce802614118df1a |
| 출처 메모 | uspto-grants-2006_03 |