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Hydrochloric Acid → HCID 178484724、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | HCID 178478588 | HCID 178478588 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178484724 | HCID 178484724 | 143.6% |
反応手順
0.56 g (1.2 mmol) trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride was suspended in dry dichloromethane (50 ml), triethylamine 0.77 ml, 6 mmol) was added and 0.13 g (0.44 mmol) triphosgene dissolved in dichloromethane was dropped in. After one hour stirring at room temperature dimetilamine hydrochloride (0.49 g, 6 mmol) followed by triethylamine (0.84 ml, 6 mmol) was added and the stirring was continued for 20 hours. The mixture was filtered, the filtrate washed with water, dried and evaporated in vacuo. Recrystallizing the product from methanol gave the title compound (0.27 g, 52%). Melting point: 212-4° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737142B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-258c082de91b464ba0230efdebd317cf |
| 出典メモ | uspto-grants-2010_06 |