関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | 4,4-Diphenylcyclohexanone | HCID 138281 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-[4,4-Diphenylcyclohexylamino]ethylamine | HCID 21998656 | 100% |
反応手順
A mixture of 4,4-diphenylcyclohexanone (2.5 g) and ethylenediamine (10 g) and p-toluenesulfonic acid (100 mg) in benzene (200 mL) was refluxed for 4 h in Dean-Stark trap to remove the water that formed. Solvent was evaporated and the residue was redissolved in methanol (60 mL) and cooled to 0° C. To this, sodium borohydride (2 g) was added in portions and the mixture was stirred at room temperature for 3 h. Solvent was evaporated, the residue was dissolved in dichloromethane (300 mL), washed with brine (3×500 mL), dried (potassium carbonate), and the solvent evaporated to leave the product as a colorless viscous oil (2.94 g, 100%). The 1H-NMR showed this product to be pure and was used in the next step without any further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06172066B2 |
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| 出典データセット | uspto-grants-2001_01 |
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| ORD ID | ord-60c6cc833e5f4589bd21a830ae47c16c |
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| 出典メモ | uspto-grants-2001_01 |
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