Reaktion #1669413

Reaktionsgleichung

sodium hydroxide

2-[2-[[[Amino(imino)methyl]amino]carbonyl]-1-methyl-4-(trifluoromethyl)-1H-indol-6-yl]ethylphosphonic acid hydrobromide

sodium hydroxide

hydrochloric acid

→

2-[2-[[[amino(imino)methyl]amino]carbonyl]-1-methyl-4-(trifluoromethyl)-1H-indol-6-yl]-ethylphosphonic acid

Ausbeute 96.2%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONby adding
2. 2
   workup.DISSOLUTIONdissolution
3. 3
   FiltrationThe resulting solution was filtered
4. 4
   Sonstigethe white solid precipitated
5. 5
   Filtrationwas collected by filtration
6. 6
   SonstigeThe white solid obtained
7. 7
   Waschenwas washed with water
8. 8
   Sonstigedried under reduced pressure

Vorschrift

2-[2-[[[Amino(imino)methyl]amino]carbonyl]-1-methyl-4-(trifluoromethyl)-1H-indol-6-yl]ethylphosphonic acid hydrobromide (2.34 g, 4.24 mmol) was suspended in distilled water (100 ml), followed by adding thereto a 1.0N aqueous sodium hydroxide solution (12.7 ml, 12.7 mmol) to effect dissolution and adjust the pH to 11. The resulting solution was filtered and the filtrate was adjusted to a pH of 1 or lower with a 1.0N aqueous hydrochloric acid solution (8.48 ml, 8.48 mmol). After confirming that the filtrate became a white suspension, the filtrate was adjusted to pH 5 with a 1.0N aqueous sodium hydroxide solution and the white solid precipitated was collected by filtration. The white solid obtained was washed with water and then dried under reduced pressure to obtain 1.60 g of 2-[2-[[[amino(imino)methyl]amino]carbonyl]-1-methyl-4-(trifluoromethyl)-1H-indol-6-yl]-ethylphosphonic acid as a white solid.

Quelle