関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | 4-(4'-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-methylaminomethylphenyl)benzamide | HCID 22010845 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 4-(4'-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-dimethylaminomethylphenyl)benzamide | HCID 22010792 | 41% |
反応手順
To a solution of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-methylaminomethylphenyl)benzamide (154 mg) in a mixture of methanol (10 ml) and acetic acid (0.5 ml) were added aqueous formaldehyde (0.2 ml) and sodium cyanoborohydride (20.9 mg) and the solution was stirred at ambient temperature for 4 hours. The mixture was diluted with chloroform and the solution was washed with saturated aqueous sodium hydrogen carbonate and brine. The organic phase was dried over magnesium sulfate and the solvent was evaporated in vacuo to give crude oil. The oil was purified by silica gel column (10 g, 2% methanol in chloroform) and the product was solidified with diethyl ether to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-dimethylaminomethylphenyl)benzamide (65 mg) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211242B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-7f02cd0acf134e0d9b4a99198696aa62 |
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| 出典メモ | uspto-grants-2001_04 |
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