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Methanesulfonic Acid → 1,4-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 1,4-Bis[5-(3,4,5-trimethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine | HCID 20634924 | — |
| 溶媒 | Chloroform ethanol | HCID 21889567 | — |
| 生成物 | 1,4-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate | HCID 20634923 | — |
反応手順
To a solution of 1,4-bis[5-(3,4,5-trimethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (72.4 g, 0.120 mol) in ethanol-chloroform (1:3, 600 mL) was added methanesulfonic acid (24.9 g, 0.258 mol), and the reaction mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a slightly yellow crystalline powder (melting point: 204.0-206.0° C.) (88.2 g, yield: 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706703B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-780fc6867ddc4e848145f2500a1a1acc |
| 出典メモ | uspto-grants-2004_03 |