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Sodium Bicarbonate → 5-{3-[N-(4-Methylphenethyl)-N-methylamino]propionyl}-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Methylphenethyl bromide | HCID 570680 | — |
| 反応物 | 5-(3-Methylaminopropionyl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one | HCID 20802897 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-{3-[N-(4-Methylphenethyl)-N-methylamino]propionyl}-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one | HCID 53993990 | — |
反応手順
A mixture of 5-(3-methylaminopropionyl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one (0.20 g) (J. Med. Chem., 1963, 6, 255), 4-methylphenethyl bromide (0.14 g) and sodium hydrogen carbonate (60 mg) in acetonitrile (20 ml) was heated under reflux for 16 hours and evaporated. The residue was partitioned between water and dichloromethane and the organic layer washed with brine, dried over MgSO4 and evaporated. The residue was purified by chromatography on silica using dichloromethane plus 0-20% methanol as eluant. Appropriate fractions were combined and evaporated and the residue crystallised from ether to give the title compound as a colourless solid, 60 mg (21%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05418229 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-f317d4907b7246d2bd8a17afb1447994 |
| 出典メモ | uspto-grants-1995_05 |