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Ammonia → 3,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 3,3-Dimethyl-1,5-dioxaspiro(5.5)undecan-9-one | HCID 587968 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamine | HCID 59970317 | — |
反応手順
A solution of 20.0 g (0.1 mol) of 3,3-dimethyl-1,5-dioxaspiro[5.5]undecan-9-one in 250 ml of methanol which contained 38 g of ammonia was hydrogenated at 100° C. and a hydrogen pressure of 100 bar in the presence of 3 g of Raney nickel. The catalyst was filtered off and the solvent was stripped off in vacuo. The crude product was purified by means of a thin film evaporator (140° C./0.8 bar). This gave 16 g (80% of theory) of distillate which solidified upon standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05859009 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-1f876b8756394ccf8b294e4ac8acb593 |
| 出典メモ | uspto-grants-1999_01 |