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Ammonia → Tricyclo(5.2.1.0,2,6)decan-8-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 4,7-Methano-5H-inden-5-one, octahydro- | HCID 96509 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Tricyclo(5.2.1.0,2,6)decan-8-amine | HCID 86760 | — |
反応手順
A solution of 15 g of tricyclo[5,2,1,02,6]decan-8-one in 60 ml of methanol, which had been saturated beforehand at 10° C. with NH3, was, after addition of Raney nickel, hydrogenated in an autoclave at 90° C. and a hydrogen pressure of 100 bar for 10 hours. The catalyst was filtered off and the solvent was distilled off under reduced pressure, and the mixture was then made strongly alkaline using 10 N NaOH and extracted 2-3 times with ethyl acetate or with diisopropyl ether. The combined organic phases were dried and subjected to fractional distillation under reduced pressure. Bp6-7mm 86-88° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06825231B2 |
| 出典データセット | uspto-grants-2004_11 |
| ORD ID | ord-50cf7a5f055241dbbd55c2055c98f7b9 |
| 出典メモ | uspto-grants-2004_11 |