反应详情

A stirred solution of 3.9 g (0.015 mole) of 3-(2-chloro-6-methylphenoxy)-1-azetidinecarbonyl chloride in 20 mL of tetrahydrofuran was treated all at once with 5.1 mL (0.045 mole) of 40% aqueous dimethylamine. After stirring for 72 h the raction mixture was diluted with 200 mL of water and the oil which separated was extracted into methylene chloride (3×30 mL). The combined extracts were dried by filtering through Whatman PS paper and concentrated in vacuo (3.6 g). The crude oil solidified when cooled in a dry ice/acetone bath and was recrystallized from ethyl ether in a dry ice-acetone bath yielding, after filtering cold, 2.6 g (64.5%) of coarse white crystals, mp 46°-47° C.

1. customthe oil which separated
2. extractionwas extracted into methylene chloride (3×30 mL)
3. customThe combined extracts were dried
4. filtrationby filtering through Whatman PS paper
5. concentrationconcentrated in vacuo (3.6 g)
6. temperaturecooled in a dry ice/acetone bath
7. customwas recrystallized from ethyl ether in a dry ice-acetone bath
8. customyielding
9. filtrationafter filtering cold