反応 #2195467

反応方程式

2-[ethyl(phenyl)amino]-N,N,N-trimethylethanaminium bromide

hydrochloric acid

sodium hydroxide

2-amino-4,5-dimethyl-1,3-thiazol hydrochloride

nitrosyl sulphuric acid

→

2-[{4-[(4,5-dimethyl-1,3-thiazol-2-yl)diazenyl]phenyl}(ethyl)amino]-N,N,N-trimethylethanaminium bromide

収率 68.4%

溶媒

acetic acid

acetic acid

sulphuric acid

反応条件

後処理

1. 1
   その他rises up to 30° C
2. 2
   その他was prepared
3. 3
   その他does not exceed 5° C
4. 4
   workup.STIRRINGThe solution is further stirred for 2 hours at room temperature
5. 5
   ろ過The resulted precipitate is filtered off
6. 6
   洗浄washed with water
7. 7
   その他dried in vacuum at 40° C
8. 8
   その他After recrystallization in ethanol/water

実験手順

11.5 g 2-amino-4,5-dimethyl-1,3-thiazol hydrochloride is dissolved in a mixture of 300 ml acetic acid and 10.2 g sulphuric acid while the temperature rises up to 30° C. The mixture is cooled to 15° C. followed by dropwise addition of 33.2 g 40% aqueous nitrosyl sulphuric acid and is stirred for 1.5 hours. In a separate beaker a solution of 20 g 2-[ethyl(phenyl)amino]-N,N,N-trimethylethanaminium bromide in a mixture of 80 ml acetic acid, 8.3 g hydrochloric acid and 120 g ice was prepared. The previously prepared diazonium salt solution was added slowly to this solution so that the temperature does not exceed 5° C. The solution is further stirred for 2 hours at room temperature. The pH value is adjusted to 4 by adding an appropriate amount of 30% aqueous sodium hydroxide. The resulted precipitate is filtered off, washed with water, and dried in vacuum at 40° C. After recrystallization in ethanol/water, 20.3 g of 2-[{4-[(4,5-dimethyl-1,3-thiazol-2-yl)diazenyl]phenyl}(ethyl)amino]-N,N,N-trimethylethanaminium bromide is obtained as red crystals.

出典