反应详情

温度

70 °C

Combine methyl 2-methylthio-5-aminobenzoate (2.18 g, 11.1 mmol) and triethyl orthoformate (7.4 mL, 44.3 mmol) in glacial acetic acid (20 mL). After the formation of a yellow solid, add glacial acetic acid (40 mL). After 50 minutes, add sodium azide (2.9 g, 44.3 mmol). Heat to 70° C. After 2 hours, cool the reaction mixture to ambient temperature and stir. After 56 hours, cool in an ice bath and dilute with water (400 mL) to give a solid. After 1 hour, collect the solid by filtration, rinse with water, and dry to give methyl 2-methylthio-5-(1H-tetrazol-1-yl)benzoate: Rf=0.90 (silica gel, 10% methanol/ethyl acetate).

1. waitAfter 2 hours
2. temperaturecool the reaction mixture to ambient temperature
3. waitAfter 56 hours
4. temperaturecool in an ice bath
5. customto give a solid
6. waitAfter 1 hour
7. customcollect the solid
8. filtrationby filtration
9. washrinse with water
10. customdry