반응 #88919

반응 방정식

diethylazodicarboxylate

5-(5-Amino-3-tert-butyl-pyrazol-1-yl)-2-chloro-phenol

2-(tetrahydro-pyran-2-yloxy)-ethanol

Ph3P

→

title compound

수율 89.0%

5-tert-Butyl-2-{4-chloro-3-[2-(tetrahydro-pyran-2-yloxy)-ethoxy]-phenyl}-2H-pyrazol-3-ylamine

수율 89.0%

용매

THF

반응 조건

후처리

1. 1
   농축the mixture concentrated in vacuo
2. 2
   기타The residue was purified by FCC

실험 절차

To a solution of 5-(5-Amino-3-tert-butyl-pyrazol-1-yl)-2-chloro-phenol (WO2011/154734A1, which is incorporated herein by reference, 340 mg, 1.28 mmol), 2-(tetrahydro-pyran-2-yloxy)-ethanol (0.26 mL, 1.92 mmol) and Ph3P (671 mg, 2.56 mmol) in dry THF (10 mL) was added diethylazodicarboxylate (0.41 mL, 2.56 mmol) and the mixture stirred for 10 min. Water (4 drops) was added and the mixture concentrated in vacuo. The residue was purified by FCC, using 0-50% EtOAc in cyclohexane, to give the title compound (450 mg, 89%). LCMS (Method 3): Rt 3.73 min, m/z 394 [MH+].

출처