Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Picrate | HCID 8577 | — |
| Reactant | Diammonium hydrogen phosphate | HCID 24540 | — |
| Reactant | Sulfolane | HCID 31347 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2,4,6-Trinitroaniline | HCID 10271 | 88% |
Reaction Steps
Ammonium picrate (2.45 g, 9.95 mmol), diammonium hydrogen phosphate (13.2 g, 100 mmol) and dry sulfolane (40 ml) are placed in a glass-lined, stainless steel reactor to form a 0.25 M concentration reaction slurry. The reactor is sealed and the reaction slurry is stirred with heating for 2 hr as the temperature increases from 25 to 175° C. (40 psi pressure). The temperature is maintained at 175° C. and stirring is continued for an additional 20 hr. The cooled reaction mixture is mixed with water (400 ml) and the insoluble material is collected, washed with water and dried to give 1.99 g picramide obtained in 88% yield (Table 2, entry 3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07057072B2 |
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| Source dataset | uspto-grants-2006_06 |
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| ORD ID | ord-9e8d6a59f5c64fa086058f77aeea49b2 |
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| Source note | uspto-grants-2006_06 |
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