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Diethyl Ether → 1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(4-fluorobenzyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-phenylpyrrolidine methanesulfonic acid salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(4-fluorobenzyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-phenylpyrrolidine | HCID 9874822 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(3,4,5-Trimethoxybenzoyl)-3-(2-(4-(1-(4-fluorobenzyl)-1h-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-phenylpyrrolidine methanesulfonic acid salt | HCID 22009142 | — |
反応手順
Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(4-fluorobenzyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-phenylpyrrolidine (0.45 g) and ethyl acetate (35 mL). Add dropwise a solution of methanesulfonic acid (0.24 g, 2.6 mmol) in ethyl acetate (2.5 mL). After 18 hours, add diethyl ether (100 mL) to form a solid. Repeatedly, decant solvent and add diethyl ether. Again, decant solvent, add diethyl ether, and evaporate in vacuo to give a solid. Dry the solid in vacuo at 82° C. to give the title compound: mp; 131-136° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06211199B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-20f9ff33f36349a7825a161fa977c597 |
| 出典メモ | uspto-grants-2001_04 |