Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 2,3-Dimethylphenol | HCID 10687 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 1-tert-Butyl-3-hydroxyazetidine | HCID 287986 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | Xibenolol | HCID 146256 | — |
Reaktionsschritte
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 potassium hydroxide was added, and the mixture was heated at 155° C. for 20 hours. The reaction mixture was cooled and then dissolved in 100 parts of ether. The solution was washed three times with 50 parts of 2N-sodium hydroxide aqueous solution and extracted three times with 2N-hydrochloric acid aqueous solution. The extract was washed with 50 parts of ether and was made alkaline by adding 2N-sodium hydroxide solution gradually thereto. Then, the ether extraction was conducted three times and the extract was condensed and allowed to stand in a cool place. As a result crystals were formed, which were recrystallized twice from ether to yield 8.3 parts of 1-(2',3'-dimethylphenyloxy)-3-(tert.-butylamino)-2-propanol having a melting point of 57° C. Results of infra-red spectrum analysis and ultraviolet ray absorption analysis of the product are as follows:
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US04018824 |
|---|
| Quelldatensatz | uspto-grants-1977_04 |
|---|
| ORD ID | ord-ea1fad422f424c9cbbaeb0564efd0ab2 |
|---|
| Quellennotiz | uspto-grants-1977_04 |
|---|