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1,1'-Carbonyldiimidazole → Ngb-2849
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | 2-Anthracenecarboxylic Acid | HCID 101325 | — |
| 反応物 | 1-Piperazinebutanamine, 4-(2,3-dichlorophenyl)- | HCID 11098669 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ngb-2849 | HCID 15411150 | 80.3% |
反応手順
A mixture of 2-anthracenecarboxylic acid (100 mg, 0.45 mmol) and 1,1'-carbonyldiimidazole (82 mg, 0.5 mmol) in 10 mL of anhydrous tetrahydrofuran is stirred for 8 hours. A solution of 4-[4-(2,3-dichlorophenyl)-1-piperazinyl]-1-aminobutane (150 mg, 0.5 mmol) in 1 mL of tetrahydrofuran is added and the resulting mixture is stirred for 30 minutes. The reaction mixture is partitioned between ethyl acetate and water. The organic layer is washed with aqueous Na2CO3, dried (Na2SO4) and concentrated in vacuo to give the title compound (183 mg, 80%). The hydrochloride salt is prepared by treating the free base with ethyl acetate-HCl. The hydrochloride salt of the tide compound has a melting point of 245-247° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06025493 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-9020199858d241a18909e28ff02d8aea |
| 出典メモ | uspto-grants-2000_02 |