반응 #73970

반응 방정식

(E)-ethyl 3-(4-(4-(N-(2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethyl)sulfamoyl)phenoxy)-3,5-difluorophenyl)-2-methylacrylate

trimethylphosphine

→

title compound

수율 101.0%

(E)-ethyl 3-(4-(4-(N-(2-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)ethyl)sulfamoyl)phenoxy)-3,5-difluorophenyl)-2-methylacrylate

수율 101.0%

용매

THF

water

반응 조건

후처리

1. 1
   기타the solvents were removed at reduced pressure
2. 2
   workup.DISSOLUTIONThe residue was dissolved in water (5 mL)
3. 3
   추출extracted with EtOAc (3×25 mL)
4. 4
   건조The combined organic layers were dried (Na2SO4)
5. 5
   농축concentrated

실험 절차

To a solution of (E)-ethyl 3-(4-(4-(N-(2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethyl)sulfamoyl)phenoxy)-3,5-difluorophenyl)-2-methylacrylate (169 mg, 0.28 mmol) in THF (6 ml) and water (0.6 mL) under nitrogen was added trimethylphosphine (26 mg, 0.34 mmol). After stirring for 3 hours, the solvents were removed at reduced pressure and. The residue was dissolved in water (5 mL) and extracted with EtOAc (3×25 mL). The combined organic layers were dried (Na2SO4) and concentrated to give the title compound (162 mg).

출처