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Sodium metaborate → 4-{N-[4-(3-nitrophenyl)-2-butyl]-aminomethyl}-2,2-dimethylchroman
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium metaborate | HCID 145326 | — |
| 反応物 | 2,2-Dimethyl-3,4-dihydro-2H-1-benzopyran-4-carbaldehyde | HCID 13537043 | — |
| 反応物 | 4-(3-Nitrophenyl)butan-2-amine | HCID 13537044 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-{N-[4-(3-nitrophenyl)-2-butyl]-aminomethyl}-2,2-dimethylchroman | HCID 13537045 | — |
反応手順
12.1 g (0.1 mol) of 2-amino-4-(3-nitrophenyl)butane are added to 19.0 g (0.1 mol) of 2,2-dimethyl-4-formyl-chroman in 100 ml of methanol at 20° C., with stirring and slight cooling, and the mixture is stirred for 1.5 hours. Thereafter, 4.5 g of sodium boranate are added, and stirring is continued for 1 day, and the mixture is evaporated down and worked up with ethyl acetate/water. The ethyl acetate phase is washed with water, dried and evaporated down. Distillation gives 4-{N-[4-(3-nitrophenyl)-2-butyl]-aminomethyl}-2,2-dimethylchroman. B.p.: 225°-235° C./0.04 mmHg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04659737 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-551240f347614c54874b79a1bb7ff07d |
| 出典メモ | uspto-grants-1987_04 |