反应详情

温度

155 °C

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:

1. additionwas added
2. temperatureThe reaction mixture was cooled
3. washThe solution was washed three times with 50 parts of 2N-sodium hydroxide aqueous solution
4. extractionextracted three times with 2N-hydrochloric acid aqueous solution
5. washThe extract was washed with 50 parts of ether
6. additionby adding 2N-sodium hydroxide solution gradually
7. extractionThen, the ether extraction
8. customcondensed
9. customAs a result crystals were formed
10. customwhich were recrystallized twice from ether