反应详情

A solution of 8.34 g (0.12 mol) of hydroxylamine hydrochloride in 125 ml of water was mixed with 100 ml of methylenechloride. Solid sodium carbonate (50 g) was added with cooling. With stirring, a solution of 16.5 g (0.079 mol) of chromone-3-carbonylchloride in 250 ml of methylene chloride was added over a period of 5 minutes, keeping the temp. at 15° with ice bath cooling. After 15 minutes reaction time the thick mixture was filtered and washed with 200 ml of ice-water. The damp filter cake was recrystallized from 100 ml of water, wt 1.5 g (8.4%); mp > 300°.

1. temperaturewith cooling
2. temperatureat 15° with ice bath cooling
3. customAfter 15 minutes reaction time the thick mixture
4. filtrationwas filtered
5. washwashed with 200 ml of ice-water
6. customThe damp filter cake was recrystallized from 100 ml of water, wt 1.5 g (8.4%)