Reaktion #435819

Reaktionsgleichung

DCC

HOBt

compound

4-{[bis(1-methyl-1H-imidazol-2-ylmethyl)amino]methyl}-benzoic acid

compound

N,N-dipropylbutane-1,4-diamine

→

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

Lösungsmittel

DMF

DMF

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe whole was stirred for 15 hours
2. 2
   workup.DISTILLATIONwas distilled off
3. 3
   workup.DISSOLUTIONthe residue was then dissolved in chloroform
4. 4
   Extraktionfollowed by extraction with 1 mol/l hydrochloric acid
5. 5
   workup.ADDITIONThe aqueous layer was added with a 1 mol/l sodium hydroxide aqueous solution
6. 6
   Extraktionextracted with chloroform
7. 7
   TrocknenThe extract was dried with anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONthe solvent was then distilled off
9. 9
   workup.ADDITIONby treating with hydrochloric acid
10. 10
    SonstigeSubsequently, the treated product was purified through silica gel column chromatography (chloroform/methanol/water)

Vorschrift

The compound (75.0 mg) obtained in Example 40-1 was dissolved in DMF (2.0 ml) and then added with DCC (46.0 mg) and HOBt (36.0 mg), followed by stirring for 6 hours. A solution of the compound (76.0 mg) obtained in Example 1-2 in DMF was added to the reaction system and then the whole was stirred for 15 hours. After completion of the reaction, DMF was distilled off and the residue was then dissolved in chloroform, followed by extraction with 1 mol/l hydrochloric acid. The aqueous layer was added with a 1 mol/l sodium hydroxide aqueous solution and then extracted with chloroform. The extract was dried with anhydrous magnesium sulfate and the solvent was then distilled off, followed by treating with hydrochloric acid. Subsequently, the treated product was purified through silica gel column chromatography (chloroform/methanol/water), thereby obtaining hydrochloride (23.9 mg) of the subject compound as a white solid.

Quelle