반응 #319500

반응 방정식

sodium hydride

4-(1H-imidazol-1-yl)phenol

2-chloro-N,N-dibenzylethanamine hydrochloride

sodium iodide

→

title compound

2-[4-(1H-Imidazol-1-yl)phenoxy]-N,N-bis(phenylmethyl)-ethanamine dihydrochloride

용매

dimethylformamide

반응 조건

후처리

1. 1
   온도maintaining the temp below 10° C
2. 2
   workup.ADDITIONAfter addition
3. 3
   온도Heat
4. 4
   기타the reaction to 50° C. for 24 hr
5. 5
   기타After this time, quench with 15 mL H2O
6. 6
   여과filter
7. 7
   기타remove the solvents
8. 8
   workup.DISSOLUTIONDissolve the residue in methanolic HCl
9. 9
   기타remove the solvents

실험 절차

To a cold suspension of 33 g (0.82 mol) 50% sodium hydride in 500 mL dimethylformamide, add 50.4 g (0.315 mol) 4-(1H-imidazol-1-yl)phenol portionwise, maintaining the temp below 10° C. After addition, stir at room temp for 1 hr. Add 93.2 (0.315 mol) 2-chloro-N,N-dibenzylethanamine hydrochloride portionwise followed by 2.35 g (0.16 mol) sodium iodide. Heat the reaction to 50° C. for 24 hr. After this time, quench with 15 mL H2O, filter, and remove the solvents. Dissolve the residue in methanolic HCl and remove the solvents to provide the title compound which can be recrystallized from isopropanol.

출처