반응 #833509

반응 방정식

N,N-dimethyl-4-[1,3-thiazol-2-yldiazenyl]aniline

1,3-propane sultone

tetrahydrofuran

→

3-(2-{[4-(dimethylamino)phenyl]diazenyl}-1,3-thiazol-3-ium-3-yl)-1-propanesulfonate

수율 99.7%

용매

1-methyl-2-pyrrolidinone

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   여과the precipitated product is filtered off
3. 3
   세척washed with acetone
4. 4
   기타dried
5. 5
   기타The resulting dye is recrystallized from methanol/ethyl acetate

실험 절차

0.5 g (1.5 mmol) of N,N-dimethyl-4-[1,3-thiazol-2-yldiazenyl]aniline are dissolved in 1-methyl-2-pyrrolidinone (NMP), and 0.9 g (7.5 mmol) of 1,3-propane sultone is added. The reaction mixture is heated at, 100° C. for 4 hours. After cooling, 20 ml of tetrahydrofuran are added to the reaction mixture and the precipitated product is filtered off, washed with acetone and dried. The resulting dye is recrystallized from methanol/ethyl acetate. 0.53 g (45% of theory) of 3-(2-{[4-(dimethylamino)phenyl]diazenyl}-1,3-thiazol-3-ium-3-yl)-1-propanesulfonate is obtained as a dark blue powder.

출처