化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl Acetate → Methyl 5-fluoro-1-benzothiophene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Methyl Thioglycolate | HCID 16907 | — |
| 反応物 | 2,5-Difluorobenzaldehyde | HCID 137663 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Methyl 5-fluoro-1-benzothiophene-2-carboxylate | HCID 22473847 | 33.89% |
反応手順
TEA (3.705 g, 36.619 mmol) was added to a solution of methyl 2-mercaptoacetate (3.293 g, 30.985 mmol) in CH3CN (12.5 mL). This was followed by the addition of 2,5-difluorobenzaldehyde (4 g, 28.169 mmol) in CH3CN (12.5 mL) and the resulting reaction mass was refluxed overnight under nitrogen atmosphere. The reaction was monitored by TLC (5% ethyl acetate in hexane). The reaction mass was concentrated under reduced pressure to obtain the crude product. Purification by column chromatography on silica gel (15% ethyl acetate in hexane) afforded 2 g of the product (33.89% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08946260B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-5e0a56d21a124533abfb1ce61d0ba034 |
| 出典メモ | uspto-grants-2015_02 |