化工社化工社 化学情報印刷レポート · 研究参考用
Sulfuric Acid → 3-(3-Cyano-thiophen-2-yl)-3-oxo-propionic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Lithium Bromide | HCID 82050 | — |
| 反応物 | 2,2-Bis(trimethylsilyl)propanedioate | HCID 22224580 | — |
| 反応物 | 3-Cyanothiophene-2-carbonyl chloride | HCID 22224749 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Isopropenyl acetate | HCID 7916 | — |
| 生成物 | 3-(3-Cyano-thiophen-2-yl)-3-oxo-propionic acid | HCID 22224915 | — |
反応手順
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 tide compound by stirring in isopropenyl acetate and conc. H2SO4 according to general procedure J (method a). Obtained as an orange solid (5.6 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07151098B2 |
| 出典データセット | uspto-grants-2006_12 |
| ORD ID | ord-3e15822884e743e184b72db97fa83ce4 |
| 出典メモ | uspto-grants-2006_12 |