반응 #214423

반응 방정식

1,5-naphthalenedisulphonic acid

1-bromo-4-chloro-1-[4-(4-chlorophenyl)-phenoxy]-3,3-dimethyl-butan-2-one

imidazole

→

4-chloro-1-[4-(4-chlorophenyl)-phenoxy]-3,3-dimethyl-1(imidazol-1-yl)-butan-2-one naphthalene-1,5-disulphonate

수율 74.6%

용매

acetone

acetonitrile

반응 조건

후처리

1. 1
   온도the mixture was heated for 40 hours
2. 2
   온도under reflux
3. 3
   농축It was then concentrated
4. 4
   workup.DISTILLATIONby distilling off the solvent in vacuo
5. 5
   세척The solution was washed three times with 100 ml of water at a time
6. 6
   건조was dried over sodium sulphate
7. 7
   농축again concentrated in vacuo
8. 8
   기타the precipitate formed
9. 9
   여과was filtered off
10. 10
    기타dried

실험 절차

20.8 g (0.05 mol) of crude 1-bromo-4-chloro-1-[4-(4-chlorophenyl)-phenoxy]-3,3-dimethyl-butan-2-one were dissolved in 120 ml of absolute acetonitrile. 12 g (0.175 mol) of imidazole were added and the mixture was heated for 40 hours under reflux. It was then concentrated by distilling off the solvent in vacuo and the residue was taken up in 300 ml of methylene chloride. The solution was washed three times with 100 ml of water at a time and was dried over sodium sulphate and again concentrated in vacuo. The residue was taken up in 100 ml of acetone and a solution of 9 g (0.038 mol) of 1,5-naphthalenedisulphonic acid in 50 ml of acetone was added. After 2 hours, the precipitate formed was filtered off and dried. 19.6 g (72% of theory) of 4-chloro-1-[4-(4-chlorophenyl)-phenoxy]-3,3-dimethyl-1(imidazol-1-yl)-butan-2-one naphthalene-1,5-disulphonate of melting point 246° C. were obtained.

출처