반응 #431174

반응 방정식

thiocarbohydrazide

2-(3-pentadecylphenoxy)butanoic acid

3-nitrobenzene boronic acid

→

desired product

수율 62.5%

4-Amino-5-mercapto-3-[1-(3-pentadecylphenoxy)propyl][1,2,4]triazole

수율 62.5%

용매

toluene

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 24 hr
3. 3
   온도The reaction was cooled
4. 4
   기타The supernatant liquid was decanted
5. 5
   workup.ADDITIONTo the residual solid was added 20 mL of acetonitrile
6. 6
   기타The solid was collected
7. 7
   세척rinsed with 5 mL of cold acetonitrile
8. 8
   기타dried in vacuo

실험 절차

To a mixture of 2.65 g (25 mmol) of thiocarbohydrazide and 9.77 g (25 mmol) of 2-(3-pentadecylphenoxy)butanoic acid in 30 mL of toluene was added 0.42 g (2.5 mmol) of 3-nitrobenzene boronic acid was heated at reflux for 24 hr. The reaction was cooled and the reaction was allowed to settle. The supernatant liquid was decanted. To the residual solid was added 20 mL of acetonitrile. The mixture was stirred for 15 minutes. The solid was collected, rinsed with 5 mL of cold acetonitrile and dried in vacuo to afford 7.20 g (60.4%) of the desired product as a white solid. Analytical data are consistent with the assigned structure.

출처