반응 #347528

반응 방정식

hydrochloric acid

triethylamine

2,4,6-trimethylphenol

3-chlorosulfonyl-1,2,4-triazole

→

3-(2,4,6-trimethylphenoxysulfonyl)-1,2,4-triazole

용매

dichloromethane

반응 조건

후처리

1. 1
   온도while being cooled with ice
2. 2
   workup.STIRRINGstirred
3. 3
   workup.STIRRINGThen, the solution was stirred at room temperature for 14 hours
4. 4
   기타to separate the components
5. 5
   세척The organic layer was washed with water
6. 6
   건조it was dried with magnesium sulfate
7. 7
   기타Then, the solvent was removed by distillation
8. 8
   기타so that coarse crystals were obtained
9. 9
   기타The coarse crystals were recrystallized from n-hexane/ethyl acetate, so that 3.0 g of the titled compound
10. 10
    기타was obtained

실험 절차

4.1 g of 2,4,6-trimethylphenol was dissolved in 15 ml of dichloromethane, and 4.2 ml of triethylamine was added while stirring the solution. Further, 4.6 g of 3-chlorosulfonyl-1,2,4-triazole was gradually added while being cooled with ice and stirred. Then, the solution was stirred at room temperature for 14 hours. After that, 2N hydrochloric acid was added to separate the components. The organic layer was washed with water, and then it was dried with magnesium sulfate. Then, the solvent was removed by distillation, so that coarse crystals were obtained. The coarse crystals were recrystallized from n-hexane/ethyl acetate, so that 3.0 g of the titled compound was obtained.

출처