関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Dihydroxybutanedioic Acid | HCID 875 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 5-[Methyl(2-phenylethyl)amino]-2-phenyl-2-propan-2-ylpentanenitrile | HCID 71225 | — |
| 反応物 | Diisobutylaluminumhydride | HCID 21225700 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 2-[3-[(Phenylethyl)methylamino]-propyl]-2-isopropylphenylacetaldehyde | HCID 88638019 | — |
反応手順
180 ml of a 1M solution of diisobutylaluminum hydride in hexane were added dropwise, at -5° C., to a solution of 33.4 g (0.1 mole) of 2-[3-[(phenylethyl)-methylamino]-propyl]-isopropylphenylacetonitrile in 400 ml of diethyl ether. The mixture was stirred for 1.5 hours, after which 500 ml of 10% strength sulfuric acid were added. 30 g of tartaric acid were introduced, the mixture was rendered alkaline with concentrated potassium hydroxide solution, and the ether phase was separated off and washed several times with sodium chloride solution. After the ether phase had been dried over sodium sulfate, the ether was distilled off, the remaining oily residue was dissolved in 300 ml of ethyl acetate, and hydrochloric acid in isopropanol was added. The mixture was left to stand overnight, after which the precipitated hydrochloride was filtered off under suction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04723039 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-9e27edb996dc4b2e8698c669aeab451a |
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| 出典メモ | uspto-grants-1988_02 |
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