Reaktion #435878

Reaktionsgleichung

compound

4-{[bis(1H-imidazol-2-ylmethyl)-amino]-methyl}-N-(4-dipropylaminomethylphenyl)-benzamide

n-hexyl chloroformate

triethylamine

→

compound

4-{[bis(1-hexyloxycarbonyl-1H-imidazol-2-ylmethyl)-amino]-methyl}-N-(4-dipropylaminomethylphenyl)-benzamide

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter completion of the reaction
2. 2
   workup.DISTILLATIONthe solvent was distilled off
3. 3
   workup.ADDITIONThe residue was added with chloroform
4. 4
   Waschenwashed with water and saturated saline solution
5. 5
   Trocknendried with anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONby distilling the solvent off
7. 7
   SonstigeSubsequently, the residue was purified through silica gel column chromatography (chloroform/methanol)

Vorschrift

The compound obtained in Example 19-3 was treated with an anion-exchange resin. The treated product was dissolved in chloroform (4.0 ml) and added with n-hexyl chloroformate (manufactured by Tokyo Kasei Kogyo Co., Ltd.) (0.054 ml) and triethylamine (0.060 ml), followed by stirring at room temperature for 16 hours. After completion of the reaction, the solvent was distilled off. The residue was added with chloroform, washed with water and saturated saline solution, and dried with anhydrous sodium sulfate, followed by distilling the solvent off. Subsequently, the residue was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (66.6 mg) as a white solid.

Quelle