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Bis(2-chloroethyl) ether → 5-Morpholinobenzo[b]thiophene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bis(2-chloroethyl) ether | HCID 8115 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzo(b)thiophen-5-amine | HCID 288032 | — |
| 生成物 | 5-Morpholinobenzo[b]thiophene | HCID 13922906 | 69.3% |
反応手順
5-Aminobenzo[b]thiophene (5.4 g, 0.0362 mole), bis-(2-chloroethyl)ether (5.2 g, 0.0364 mole) and 40% aqueous NaOH (0.073 mole) were stirred vigorously and heated to refluxing for 22 hours. The cooled mixture was extracted with CHCl3. Evaporation of the washed and dried CHCl3 extract under reduced pressure left 7.0 g (88%) of the crude product as a slightly oily, dark yellow solid. This material was combined with 1.75 g of comparable crude product from a previous run. Recrystallization from CH3CN afforded 5.50 g of 5-morpholinobenzo[b]thiophene, m.p. 127°-132° C., that was characterized by nmr.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04668697 |
| 出典データセット | uspto-grants-1987_05 |
| ORD ID | ord-c26d72fc650d46f6ba647da085ccbccc |
| 出典メモ | uspto-grants-1987_05 |