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Sodium Carbonate → 3,4-dihydrobenzothieno[2,3-c]-pyridine-2(1H)-butanenitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4-Chlorobutyronitrile | HCID 12336 | — |
| 反応物 | 1,2,3,4-Tetrahydro[1]benzothieno[2,3-c]pyridine | HCID 413282 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3,4-dihydrobenzothieno[2,3-c]-pyridine-2(1H)-butanenitrile | HCID 18378958 | 101.4% |
反応手順
A mixture of 1,2,3,4-tetrahydro-[1]benzothieno[2,3-c]pyridine (0.02 mol), Na2CO3 (5 g), KI (0.1 g) and 4-chlorobutanenitrile (0.025 mol) in acetonitrile (50 ml) and methylbenzene (150 ml) was stirred and refluxed overnight, then cooled, filtered and the filtrate was evaporated. The residue (oil) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2). The pure fractions were collected and the solvent was evaporated, yielding 5.2 g of 3,4-dihydrobenzothieno[2,3-c]-pyridine-2(1H)-butanenitrile (interm. 6).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06495555B1 |
| 出典データセット | uspto-grants-2002_12 |
| ORD ID | ord-fde6fc8e3ab44b2f98e46e198b471392 |
| 出典メモ | uspto-grants-2002_12 |