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Morpholine → 4-[4-(Methylthio)benzoyl]morpholine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 4-(Methylthio)benzoic acid | HCID 83230 | — |
| 反応物 | N-[2-(dimethylamino)ethyl]-N'-ethylcarbodiimide hydrochloride | HCID 57494384 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-[4-(Methylthio)benzoyl]morpholine | HCID 25572261 | — |
反応手順
To a stirred solution of 4-(methylthio)benzoic acid (6.76 g, 40.2 mmol) and N-[2-(dimethylamino)ethyl]-N′-ethylcarbodiimide hydrochloride (9.24 g, 48.2 mmol) in THF (100 mL) was added morpholine (4.2 mL, 48.2 mmol). After stirring for 2 hours, the reaction was concentrated in vacuo and the residue partitioned between ethyl acetate (100 mL) and 2M hydrochloric acid (150 mL). The organic phase was separated, washed with 1M aqueous sodium carbonate solution, dried over sodium sulfate, filtered and concentrated in vacuo to give the title compound LC retention time 3.52 mins MS m/z 238 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07446117B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-037be1b1b0ef41ba93b21ed6ef1338dd |
| 出典メモ | uspto-grants-2008_11 |