反应详情

A solution of sodium azide (4.14 g.) in water (16 ml.) was added dropwise to a solution of 2-tetrahydrothiophenecarboxylic acid chloride (9.60 g.) in diethyl ether (24 ml.) with stirring under ice-cooling and stirred for further 15 minutes at the same temperature. After the mixture was stirred for 1 hour at ambient temperature, nitrogen gas was introduced to remove off diethyl ether. The resultant mixture was extracted with diethyl ether (50 ml.). The extracts were washed with water, dried over magnesium sulfate and concentrated in vacuo to give oily 2-tetrahydrothiophenecarboxylic acid azide (8.63 g.).

1. temperaturecooling
2. stirringstirred for further 15 minutes at the same temperature
3. stirringAfter the mixture was stirred for 1 hour at ambient temperature
4. additionnitrogen gas was introduced
5. customto remove off diethyl ether
6. extractionThe resultant mixture was extracted with diethyl ether (50 ml.)
7. washThe extracts were washed with water
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated in vacuo