Reaktion #1074202

Reaktionsgleichung

1-(4-nitrophenyl)piperazine

3,5-di-tert-butyl-4-hydroxybezoic acid

dicyclohexylcarbodiimide

→

2,6-bis-(1,1-dimethylethyl)-4-{[4-(4-nitrophenyl)-1-piperazinyl]-carbonyl}-phenol

Ausbeute 89.0%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationthe precipitate which appears is filtered out
2. 2
   Waschenrinsed with ethyl acetate
3. 3
   workup.ADDITIONAfter concentration of the filtrate under reduced pressure, the residue is diluted in 20 ml of ethyl acetate
4. 4
   Filtrationa new insoluble is eliminated by filtration
5. 5
   SonstigeThe solvent is evaporated off under vacuum
6. 6
   Sonstigethe residue is precipitated from diethyl ether
7. 7
   FiltrationThe solid is filtered
8. 8
   Waschenrinsed with 2×20 ml of ethyl acetate in order
9. 9
   Sonstigeto obtain a yellow powder with a yield of 89%

Vorschrift

2.07 g (10 mmoles) of 1-(4-nitrophenyl)piperazine, 2.5 g (10 mmoles) of 3,5-di-tert-butyl-4-hydroxybezoic acid and 2.26 g (11 mmoles) of dicyclohexylcarbodiimide are introduced into a 100 ml flask containing 25 ml of DMF. The reaction medium is agitated for 15 hours at ambient temperature, the precipitate which appears is filtered out and rinsed with ethyl acetate. After concentration of the filtrate under reduced pressure, the residue is diluted in 20 ml of ethyl acetate and a new insoluble is eliminated by filtration. The solvent is evaporated off under vacuum and the residue is precipitated from diethyl ether. The solid is filtered, rinsed with 2×20 ml of ethyl acetate in order to obtain a yellow powder with a yield of 89%. Melting point: 159.5-160.5° C.

Quelle