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Sulfuric Acid → 3-(3-Chloro-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 | Acetonitrile | HCID 6342 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Lithium Bromide | HCID 82050 | — |
| 反応物 | 3-Chlorothiophene-2-carbonyl chloride | HCID 2735824 | — |
| 反応物 | 2,2-Bis(trimethylsilyl)propanedioate | HCID 22224580 | — |
| 溶媒 | Isopropenyl acetate | HCID 7916 | — |
| 生成物 | 3-(3-Chloro-thiophen-2-yl)-3-oxo-propionic acid | HCID 22224616 | — |
| 生成物 | 6-(3-Chloro-thiophen-2-yl)-2,2-dimethyl-[1,3]dioxin-4-one | HCID 22224775 | — |
反応手順
The 3-(3-chloro-thiophen-2-yl)-3-oxo-propionic acid was prepared from 3-chloro-thiophene-2-carbonyl chloride (7.82 g, 43.2 mmol) and bis(trimethylsilyl)malonate (11.6 mL, 45.4 mmol) with Et3N (12.65 mL, 90.7 mmol) and LiBr (3.53 g, 47.5 mmol) in CH3CN at 0° C. according to general procedure H (method c1). The crude material (5.69 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 (2.3 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-53e1892dc84943f4a75f9dfcf7a3e118 |
| 出典メモ | uspto-grants-2006_12 |