Reaktion #1259198

Reaktionsgleichung

acetic acid

2,5-dihydroxyterephthalic acid

2,3,5,6-tetraaminopyridine trihydrochloride monohydrate

2,5-dihydroxyterephthalic acid disodium salt

2,3,5,6-tetraaminopyridine trihydrochloride monohydrate

→

2,3,5,6-tetraaminopyridine

Lösungsmittel

water

sodium hydroxide

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere added
2. 2
   Sonstigethe resultant salt was recovered
3. 3
   Filtrationby filtering
4. 4
   workup.ADDITIONdispersed in, and
5. 5
   workup.ADDITIONmixed with, 3,000 parts by weight of water
6. 6
   Filtrationby re-filtering
7. 7
   workup.ADDITIONProcedures of the above dispersing/mixing
8. 8
   Filtrationfiltering

Vorschrift

17.772 Parts by weight of 2,3,5,6-tetraaminopyridine trihydrochloride monohydrate was dissolved in 100 parts by weight of water deaerated with nitrogen. 13.208 Parts by weight of 2,5-dihydroxyterephthalic acid was dissolved in 137 parts by weight of a 1M sodium hydroxide aqueous solution, followed by deaeration with nitrogen. The 2,3,5,6-tetraaminopyridine trihydrochloride monohydrate aqueous solution was dropwise added to the 2,5-dihydroxyterephthalic acid disodium salt aqueous solution over 10 minutes. Then, 24.3 parts by weight of polyphosphoric acid, 35 parts by weight of water deaerated with nitrogen and 1 part by weight of acetic acid were added, and the resultant salt was recovered by filtering and dispersed in, and mixed with, 3,000 parts by weight of water deaerated with nitrogen, followed by re-filtering. Procedures of the above dispersing/mixing and filtering were repeated 3 times to give 2,3,5,6-tetraaminopyridine/2,5-dihydroxyterephthalaic acid salt.

Quelle