反应详情

温度

0 °C

Dissolve the compound obtained in Example 2 (1.5 g) in tetrahydrofuran (20 ml). Add 2N sodium hydroxide (8 ml) to the reaction mixture, cooled to 0° C. using an ice bath. Stir magnetically at ambient temperature for 72 hours. Remove the tetrahydrofuran by evaporation under reduced pressure. Take up the resulting residue in a 6N hydrochloric acid solution to pH 1 and extract twice with 50 ml of ether each time. Dry the organic phase over magnesium sulphate and remove the ether by evaporation under reduced pressure. Crystallise the resulting oil from isopropyl ether and recrystallise the resulting precipitate from cyclohexane.

1. customRemove the tetrahydrofuran
2. customby evaporation under reduced pressure
3. extractionextract twice with 50 ml of ether each time
4. dry with materialDry the organic phase over magnesium sulphate
5. customremove the ether
6. customby evaporation under reduced pressure
7. customCrystallise the resulting oil from isopropyl ether
8. customrecrystallise the resulting precipitate from cyclohexane