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Formaldehyde → 1-(4-Morpholin-4-ylmethyl-1H-pyrrol-2-yl)-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 2-Acetylpyrrole | HCID 14079 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(4-Morpholin-4-ylmethyl-1H-pyrrol-2-yl)-ethanone | HCID 66636007 | — |
反応手順
To a solution of morpholine (22 mmoles) in acetic acid (60 ml) at 0° C. there are added 1-(1H-pyrrol-2-yl)-ethanone (20 mmoles) and formaldehyde (20 mmoles) 37% in water. The reaction mixture is stirred overnight at ambient temperature. At 0° C., the solution is brought to alkaline pH (10-12) using 20% aqueous NaOH solution and is then extracted with DCM. The organic phase is washed with water and with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness. Purification by flash chromatography on silica gel (SiO2; gradient DCM/MeOH) to yield the title product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541412B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-a85c8460d2724fbe85f1a9c59865968b |
| 出典メモ | uspto-grants-2013_09 |