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Hydrochloric Acid → 3-Dimethylamino-1-(5-methyl-2-thienyl)-propan-1-one hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | 2-Acetyl-5-methylthiophene | HCID 83655 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Dimethylamino-1-(5-methyl-2-thienyl)-propan-1-one hydrochloride | HCID 12643436 | 65.7% |
反応手順
Under a nitrogen atmosphere, a stirred solution of 10.0 grams (0.071 mole) of 2-acetyl-5-methylthiophene, 7.0 grams (0.086 mole) of dimethylamine hydrochloride, 2.5 grams of paraformaldehyde and 0.4 ml of concentrated hydrochloric acid in 10 ml of ethanol was heated under reflux for 16 hours. The reaction mixture was concentrated under reduced pressure to a residual solid. The solid was recrystallized from methanol-diethyl ether to give 10.9 grams of 3-dimethylamino-1-(5-methyl-2-thienyl)propan-1-one hydrochloride; m.p. 145°-147° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04645777 |
| 出典データセット | uspto-grants-1987_02 |
| ORD ID | ord-7533c9036b464e4a94d876df66df5f98 |
| 出典メモ | uspto-grants-1987_02 |