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N,N-Dimethylaniline → 2-(4-chlorophenyl)-4-(dimethylamino)acetyl-3,4-dihydro-2H-1,4-benzothiazine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-Dimethylaniline | HCID 949 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-(4-chlorophenyl)-3,4-dihydro2H-1,4-benzothiazine | HCID 13071524 | — |
| 反応物 | 2-(Dimethylamino)acetyl chloride hydrochloride | HCID 13994991 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(4-chlorophenyl)-4-(dimethylamino)acetyl-3,4-dihydro-2H-1,4-benzothiazine hydrochloride | HCID 19794236 | 165.5% |
反応手順
To a solution of 2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine (0.52 g) and N,N-dimethylaniline (0.97 g) in methylene chloride (15 ml) is added dimethylaminoacetyl chloride hydrochloride (0.63 g) under ice cooling, and the mixture is stirred at the same temperature for 2.5 hours. To the reaction mixture is added aqueous sodium hydrogen carbonate solution, and is extracted with chloroform. The chloroform layer is washed, dried and distilled to remove the solvent. The residue is treated with hydrochloric acid and the resulting salt is recrystallized from ethanol-ether to give 2-(4-chlorophenyl)-4-(dimethylamino)acetyl-3,4-dihydro-2H-1,4-benzothiazine hydrochloride (0.63 g, yield 86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246929 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-1147dbdc36ea4a6199a9f7a5bb454589 |
| 出典メモ | uspto-grants-1993_09 |