関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 5-tert-butyl-1-indanone O-methyloxime | HCID 73047460 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-tert-butyl-2,3-dihydro-1H-inden-1-amine | HCID 11506601 | — |
反応手順
5-tert-Butyl-1-indanone O-methyloxime (4.37 g, 20.2 mmol) and 10% palladium on carbon (2.2 g) were combined in methanol (50 ml) and ammonia (10 ml) and placed in a Parr apparatus, which was charged with hydrogen to 60 psi. The reaction was shaken at 50° C. for 16 hours. The reaction mixture was filtered and the filtrate was evaporated under reduced pressure. The residue was treated with diethyl ether (100 ml) and extracted with hydrochloric acid (1N, 3×50 ml). The combined aqueous extracts were neutralized with sodium hydroxide (6 g) in water (25 ml) and extracted with diethyl ether. The organic extracts were combined, dried with magnesium sulfate, and the filtrate was evaporated under reduced pressure to provide the title compound, which was used without further purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08487116B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-9e243e9d9646465aaec0cc424959d5bf |
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| 出典メモ | uspto-grants-2013_07 |
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