تفاعل #88919

معادلة التفاعل

diethylazodicarboxylate

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

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

Ph3P

→

title compound

المردود 89.0%

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

المردود 89.0%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   تركيزthe mixture concentrated in vacuo
2. 2
   أخرىThe residue was purified by FCC

الإجراء التجريبي

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+].

المصدر