Reaktionsgleichung
[CH3:1]S(O)(=O)=O.[OH:6][CH2:7][CH2:8][C:9]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([CH2:18][N:19]3[CH:23]=[N:22][CH:21]=[N:20]3)[CH:16]=2)[NH:11][C:10]=1[C:24]([OH:26])=[O:25]>CO>[CH3:1][O:25][C:24]([C:10]1[NH:11][C:12]2[C:17]([C:9]=1[CH2:8][CH2:7][OH:6])=[CH:16][C:15]([CH2:18][N:19]1[CH:23]=[N:22][CH:21]=[N:20]1)=[CH:14][CH:13]=2)=[O:26]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
2.7 ml (42 mmoles) of methanesulphonic acid were added to a suspension de 6 g (21 mmoles) of the 3-(2-hydroxyethyl)-5-[1,2,4]triazol-1-ylmethyl-1H-indol-2-carboxylic acid in 120 ml of methanol. The mixture was left under stirring at reflux temperature for 3 hours. The solvent was evaporated to dryness under reduced pressure, the residue dissolved with 20 ml of a saturated bicarbonate solution and extracted 3 times with ethyl acetate. The combined organic phases were dried and evaporated to dryness, and the evaporated solid recrystallised from isopropyl alcohol/heptane to give 5.9 g (93%) of the title ester as a yellow crystalline solid.
Aufarbeitung
- waitThe mixture was left
- temperatureat reflux temperature for 3 hours
- customThe solvent was evaporated to dryness under reduced pressure
- dissolutionthe residue dissolved with 20 ml of a saturated bicarbonate solution
- extractionextracted 3 times with ethyl acetate
- customThe combined organic phases were dried
- customevaporated to dryness
- customthe evaporated solid recrystallised from isopropyl alcohol/heptane
Quellen und Nachweise
- ORD-Eintrag
- ord-808bd576f9724ea895b7e69c75fc2e71
- Quelldatensatz
- uspto-grants-2007_10
- Patentnummer
- US07279581B2
Verknüpfte Notizen
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