Reaktion #951223

Reaktionsgleichung

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

fumaric acid

→

(RS)-2-(4,4,7-trimethyl-1,4-dihydroindeno[2,1-c]pyrazol-1-yl )-1-methyl-ethylamine fumarate

Ausbeute 69.0%

Lösungsmittel

diethyl ether

ethanol

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

1.1 g (3.9 mmol) of (RS)-1-(2-azido-propyl)-4,4,7-trimethyl-1,4-dihydro-indeno[2,1-c]pyrazole dissolved in 60 ml of anhydrous ethanol were hydrogenated over 110 mg of platinum oxide for 3 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 150 ml of anhydrous diethyl ether, filtered and treated while stirring with a solution of 453 mg (3.9 mmol) of fumaric acid in 10 ml of methanol. The mixture was stirred at room temperature for 4 hours and the white crystals were subsequently filtered off. 1 g (69%) of (RS)-2-(4,4,7-trimethyl-1,4-dihydroindeno[2,1-c]pyrazol-1-yl )-1-methyl-ethylamine fumarate (1:1) with m.p. 167° was obtained.

Quelle