反应详情

A solution of 1.05 g of triethylamine in 20 ml of absolute dimethoxyethane was added dropwise within 15 minutes with stirring to a mixture of 1.78 g (10 mmol) of 1-(4-hydroxyphenyl)piperazine, 2.48 g (13.5 mmol) of 2-chloromethylbenzothiazole and 80 ml of absolute 1,2-dimethoxyethane under reflux. The mixture was stirred for a further 5 hours under reflux, the solvent was evaporated in vacuo, the residue was taken up in CH2Cl2 /H2O, the phases were separated, and the aqueous phase was extracted three times with CH2Cl2. The combined CH2Cl2 extracts were dried, filtered and evaporated. The crystalline residue (3.2 g) was recrystallized from methanol. 2.64 g (81.2% of theory) of pure 1-(4-hydroxyphenyl)-4-(benzothiazol-2-ylmethyl)piperazine, melting point 175°-76° C., were obtained.

1. temperatureunder reflux
2. temperatureunder reflux
3. customthe solvent was evaporated in vacuo
4. customthe phases were separated
5. extractionthe aqueous phase was extracted three times with CH2Cl2
6. dry with materialThe combined CH2Cl2 extracts were dried
7. filtrationfiltered
8. customevaporated
9. customThe crystalline residue (3.2 g) was recrystallized from methanol