化工社化工社 化学情報印刷レポート · 研究参考用
Ethanolamine → 2,2-Dichloro-1-(8-methyl-1-oxa-4-azaspiro[4.5]decan-4-yl)ethan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanolamine | HCID 700 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloroacetyl chloride | HCID 6593 | — |
| 反応物 | 4-Methylcyclohexanone | HCID 11525 | — |
| 生成物 | 2,2-Dichloro-1-(8-methyl-1-oxa-4-azaspiro[4.5]decan-4-yl)ethan-1-one | HCID 13277204 | — |
反応手順
From a boiling mixture of 11.2 g. (0.1 moles) of 4-methyl-cyclohexanone and 6.1 g. (0.1 moles) of ethanolamine in 100 ml. of benzene the formed water is continuously distilled off. Boiling is continued until 1.8 ml. of water are separated. The reaction mixture is then cooled and 8 g. (0.1 moles) of pyridine are added followed by dropwise addition of 14.7 g. (0.1 moles) of dichloroacetyl chloride with external salt/ice cooling. Further following the procedure described in Example 2, 20.7 g. (0.078 moles) of a rose, oily product are obtained. Recrystallization from absolute ethanol affords a white, crystalline product melting at 119° to 120° C. The structure of the compound obtained can be verified by IR spectrum analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04256481 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-7e8eee49de1241f0a4981066e19cc3e7 |
| 出典メモ | uspto-grants-1981_03 |