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Hydrochloric Acid → N-(11-Amino-2,2,12-trimethyltrideca-4,8-dien-1-ylidene)hydroxylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 3,3-Dimethyl-12-isopropyl-1-aza-1,5,9-cyclododecatriene | HCID 557512 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(11-Amino-2,2,12-trimethyltrideca-4,8-dien-1-ylidene)hydroxylamine | HCID 71403854 | 92% |
反応手順
233.4 g (1 mol) of 3,3-dimethyl-12-isopropyl-1-aza-1,5,9-cyclododecatriene is added dropwise to 100 g of 37% hydrochloric acid and 200 ml of water in the course of one hour, in a manner ensuring that the temperature does not exceed 80° C. The mixture is then cooled to 20°-25° C., and 69.5 g (1.0 mol) of hydroxylamine hydrochloride is added. There is subsequently added during one hour, while cooling with a water bath, about 92 g (2.3 mols) of solid sodium hydroxide until the pH value of the aqueous solution is 10-11. The organic phase which precipitates is separated, and washed free from salt with water. Distillation yields 245 g (0.92 mol) of 2,2-dimethyl-11-isopropyl-11-amino-undeca-4,8-dienal-oxime; b.p. 158°-162° C./4 Pa; nD20 =1.4930.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04297480 |
| 出典データセット | uspto-grants-1981_10 |
| ORD ID | ord-f40c5d23cd874a4d8c7f81950515103b |
| 出典メモ | uspto-grants-1981_10 |