반응 #47197

반응 방정식

5-tert-butyl-2-aminothiophene-3-carboxylic acid

2,3-dichlorophenyl isocyanate

→

5-tert-butyl-2-(3-(2,3-dichlorophenyl)ureido)thiophene-3-carboxylic acid

수율 83.0%

용매

THF

반응 조건

후처리

1. 1
   기타The vial was capped
2. 2
   온도The reaction was cooled down to room temperature
3. 3
   기타the solvent was removed under vacuum
4. 4
   workup.ADDITIONThe oil residue was treated with dichloromethane
5. 5
   workup.WAITthe resulting mixture was left
6. 6
   workup.WAITto stand at room temperature for 1 hour
7. 7
   여과The solids were filtered
8. 8
   세척washed with minimal amount of dichloromethane
9. 9
   기타dried under vacuum

실험 절차

To a vial containing 5-tert-butyl-2-aminothiophene-3-carboxylic acid (1 mmol) in THF (7 mL) was added 2,3-dichlorophenyl isocyanate (1 mmol). The vial was capped and the solution was stirred at 70° C. for 21 hours. The reaction was cooled down to room temperature and the solvent was removed under vacuum. The oil residue was treated with dichloromethane and the resulting mixture was left to stand at room temperature for 1 hour. The solids were filtered, washed with minimal amount of dichloromethane and dried under vacuum to yield the expected 5-tert-butyl-2-(3-(2,3-dichlorophenyl)ureido)thiophene-3-carboxylic acid (317.2 mg, 83%). Coupling with the appropriate amine was performed as described above for Example 1.

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