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7.3 g (0.036 mol) Methyl 4-ethynyl-3-nitrobenzoate (Compound II-1), 300 ml methanol and 200 ml tetrahydrofuran were added into a reaction flask, stirred, and ammonia gas was passed through for 1 hour. Then the mixture was reacted at room temperature for 24 hours. After completion of the reaction monitored by TLC, the mixture was concentrated under reduced pressure with most of the tetrahydrofuran and methanol evaporated, then extracted with 300 ml ethyl acetate. The organic layer was washed with water for three times, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated to dryness, and separated by column chromatography to obtain 4-ethynyl-3-nitrobenzamide (compound I-1), 3.6 g (0.0019 mol), yield 53.2%.

1. customwas passed through for 1 hour
2. customThen the mixture was reacted at room temperature for 24 hours
3. concentrationthe mixture was concentrated under reduced pressure with most of the tetrahydrofuran and methanol
4. customevaporated
5. extractionextracted with 300 ml ethyl acetate
6. washThe organic layer was washed with water for three times
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationfiltered
9. concentrationthe filtrate was concentrated to dryness
10. customseparated by column chromatography