反应详情

Ammonium picrate (0.18 g, 0.75 mmol) and diammonium hydrogen phosphate (0.99 g, 7.5 mmol) are suspended in dry sulfolane (3 ml) and stirred in a Teflon® capped glass pressure tube (8 ml) for 2 hr with the application of heat, which raises the temperature of the reaction from 25° C. to 177° C. The reaction is continued an additional 5 hr at 177° C. and cooled to ambient temperature. Water (30 ml) is added to the slurry and the product is collected and washed with water. Vacuum drying yields 0.13 g (76%) of picramide (Table 1, entry 1).

1. customcapped glass pressure tube (8 ml) for 2 hr with the application
2. temperatureof heat
3. temperaturewhich raises
4. customthe temperature of the reaction from 25° C. to 177° C
5. customthe product is collected
6. washwashed with water
7. customVacuum drying