反应详情

0.46 g (2.87 mmol) 4-ethynyl-3-aminobenzamide (Compound XI-1), 10 ml water, were added into a 50 ml single-neck flask, then 1.2 g 58% sulfuric acid was added, and then 0.92 g 18.5% potassium dichromate solution. The mixture was stirred for 3 minutes until completing the reaction, extracted with ethyl acetate, dried over anhydrous sodium sulfate, and separated by column chromatography to obtain 0.06 g 4-ethynyl-3-nitrosobenzamide (Compound I-28, yellow-green solid), yield 12%, stored at −20° C.

1. customthe reaction
2. extractionextracted with ethyl acetate
3. dry with materialdried over anhydrous sodium sulfate
4. customseparated by column chromatography