関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Dimethylphenol | HCID 10687 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-tert-Butyl-3-hydroxyazetidine | HCID 287986 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Xibenolol | HCID 146256 | — |
反応手順
To a mixture of 6.5 parts of 1-(tert.butyl)-3-azetidinol and 6.7 parts of 2,3-xylenol 0.2 part of sodium hydroxide was added, and the mixture was heated at 160° C. for 24 hours. The reaction mixture was cooled and then dissolved in 100 parts of ether. The solution was washed twice with 50 parts of 2 N-sodium hydroxide aqueous solution and extracted three times with 50 parts of 2 N-hydrochloric acid aqueous solution. The extract was washed with 50 parts of ether and was made alkaline by addition of 2 N-sodium hydroxide aqueous solution. The solution was cooled and agitated to form crystals. The resulting crystals were dried and recrystallized twice from ether to yield 9.2 parts of 1-(2',3'-dimethylphenyloxy)-3-(tert.-butylamino)-2-propanol having a melting point of 57° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04360464 |
|---|
| 出典データセット | uspto-grants-1982_11 |
|---|
| ORD ID | ord-9600be261acb4834855eb3c0ecbd4206 |
|---|
| 出典メモ | uspto-grants-1982_11 |
|---|