反应详情

Sodium hydride (0.6 g) and 2-amino-5-diethylaminoethylthio-1,3,4-thiadiazole (2.3 g) were stirred in tetrahydrofuran (30 ml) for 30 minutes while being cooled with ice. 4-Isopropyloxybenzoic acid (1.8 g) and carbonyldiimidazole (1.8 g) were stirred in tetrahydrofuran (30 ml) for 30 minutes at room temperature and the mixture was added to the former reaction mixture. The mixture was stirred for 4 hours at room temperature, and then concentrated under a vacuum. The residue, with water added thereto, was extracted with ethyl acetate. The extract was dried over sodium sulfate anhydride, and then concentrated under a vacuum. The residue was purified by silica gel column chromatography (chloroform:methanol=20:1). The resulting solid was recrystallized from n-hexane/ethanol, thereby yielding 2.4 g of the aimed compound.

1. temperaturewhile being cooled with ice
2. additionthe mixture was added to the former reaction mixture
3. concentrationconcentrated under a vacuum
4. additionThe residue, with water added
5. extractionwas extracted with ethyl acetate
6. dry with materialThe extract was dried over sodium sulfate anhydride
7. concentrationconcentrated under a vacuum
8. customThe residue was purified by silica gel column chromatography (chloroform:methanol=20:1)
9. customThe resulting solid was recrystallized from n-hexane/ethanol