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Benzo(B)Thiophene → 2-[2-(4-Hydroxy-4-(2-benzothienyl)-piperidino)-ethyl]-1,4-benzodioxan
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzo(B)Thiophene | HCID 7221 | — |
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Lithium diisopropylamide | HCID 2724682 | — |
| 反応物 | 1-[2-(2,3-Dihydro-1,4-benzodioxin-2-yl)ethyl]piperidin-4-one | HCID 20540170 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 2-[2-(4-Hydroxy-4-(2-benzothienyl)-piperidino)-ethyl]-1,4-benzodioxan | HCID 53672426 | — |
反応手順
To lithium diisopropylamide in 50 ml of tetrahydrofuran, prepared from 2.25 ml of diisopropylamine and 10 ml of 1.6 N n-butyl lithium in hexane at -70° under nitrogen, is added 2.0 g of thianapthene in 20 ml of tetrahydrofuran while stirring. After 1 hour, the solution of 2.65 g of 2-[2-(4-oxopiperidino)-ethyl]-1,4-benzodioxan in 20 ml of tetrahydrofuran is added and, after standing overnight, the mixture is decomposed with 9 ml of saturated aqueous ammonium chloride. The organic phase is separated, dried, evaporated, the crystalline residue washed with water and recrystallized from ethanol-acetone, to yield the 2-[2-(4-hydroxy-4-(2-benzothienyl)-piperidino)-ethyl]-1,4-benzodioxan melting at 175°-178°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04140781 |
| 出典データセット | uspto-grants-1979_02 |
| ORD ID | ord-15b33e1397af4235b9515c613a1e87f9 |
| 出典メモ | uspto-grants-1979_02 |