반응 #214420

반응 방정식

naphthalenedisulphonic acid

1-bromo-4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one

1,2,4-triazole

→

4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one naphthalene-1,5-disulphonate

수율 192.6%

용매

acetone

acetonitrile

반응 조건

후처리

1. 1
   온도the mixture was heated for 20 hours
2. 2
   온도under reflux
3. 3
   농축It was then concentrated
4. 4
   workup.DISTILLATIONby distilling off the solvent in vacuo
5. 5
   세척The mixture was washed three times with 250 ml of water at a time
6. 6
   건조dried over sodium sulphate
7. 7
   농축again concentrated in vacuo
8. 8
   workup.DISSOLUTIONThe oil which remained was dissolved in 1,000 ml of acetone
9. 9
   여과the resulting precipitate was filtered off

실험 절차

268.3 g (0.79 mol) of crude 1-bromo-4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one were dissolved in 2 l of absolute acetonitrile. 190 g (2.7 mol) of 1,2,4-triazole were added thereto and the mixture was heated for 20 hours under reflux. It was then concentrated by distilling off the solvent in vacuo and the residue was taken up in 1,000 ml of methylene chloride. The mixture was washed three times with 250 ml of water at a time, dried over sodium sulphate and again concentrated in vacuo. The oil which remained was dissolved in 1,000 ml of acetone and a solution of 140 g (0.48 mol) of naphthalenedisulphonic acid in 500 ml of acetone was added. After 30 minutes, the resulting precipitate was filtered off. 285 g (76.6% of theory) of 4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one naphthalene-1,5-disulphonate of melting point 245° C. (with decomposition) were obtained.

출처