Reaktion #951218

Reaktionsgleichung

(S)-1-(2-azido-propyl)-4,4,7-trimethyl-1,4-dihydro-indeno[2,1-c]pyrazole

fumaric acid

→

(S)-2-(4,4,7-trimethyl-1,4-dihydro-indeno[2,1-c]pyrazol-1-yl)-1-methyl-ethylamine fumarate

Ausbeute 54.0%

Lösungsmittel

diethyl ether

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe catalyst was subsequently filtered off
2. 2
   Waschenrinsed with ethanol
3. 3
   Sonstigethe solvent was removed in a vacuum
4. 4
   SonstigeThe colorless oil obtained
5. 5
   Filtrationfiltered
6. 6
   workup.ADDITIONtreated
7. 7
   Filtrationthe white crystals were subsequently filtered off

Vorschrift

0.7 g (2.5 mmol) of (S)-1-(2-azido-propyl)-4,4,7-trimethyl-1,4-dihydro-indeno[2,1-c]pyrazole dissolved in 50 ml of anhydrous methanol was hydrogenated over 70 mg of platinum oxide for 2 hours. The catalyst was subsequently filtered off, rinsed with ethanol and the solvent was removed in a vacuum. The colorless oil obtained was dissolved in 70 ml of anhydrous diethyl ether, filtered and treated while stirring with a solution of 290 mg (2.5 mmol) of fumaric acid in 5 ml of methanol. The mixture was stirred at room temperature for 4 hours and the white crystals were subsequently filtered off. 0.5 g (54%) of (S)-2-(4,4,7-trimethyl-1,4-dihydro-indeno[2,1-c]pyrazol-1-yl)-1-methyl-ethylamine fumarate (1:1) with m.p. 158° was obtained.

Quelle