تفاعل #45233

معادلة التفاعل

mixture

3-(3-hydrazino-phenyl)-propionic acid ethyl ester

4,4-dimethyl-3-oxo-pentanenitrile

→

3-[3-(5-amino-3-t-butyl-pyrazol-1-yl)-phenyl]-propionic acid ethyl ester

المردود 85.2%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto reflux overnight
2. 2
   أخرىThe reaction solution was evaporated under reduced pressure
3. 3
   أخرىThe residue was purified by column chromatography

الإجراء التجريبي

A mixture of Example Y (13 g, 53.3 mmol) and 4,4-dimethyl-3-oxo-pentanenitrile (6.9 g, 55 mol) in ethanol (150 mL) was heated to reflux overnight. The reaction solution was evaporated under reduced pressure. The residue was purified by column chromatography to give 3-[3-(5-amino-3-t-butyl-pyrazol-1-yl)-phenyl]-propionic acid ethyl ester (14.3 g, 45.4 mmol) as a white solid. 1H NMR (DMSO-d6): 7.39-7.32 (m, 3H), 7.11 (d, J=6.8 Hz, 1H), 5.34 (s, 1H), 5.16 (s, 2H), 4.03 (q, J=7.2 Hz, 2H), 2.88 (t, J=7.6 Hz, 2H), 2.63 (t, J=7.6 Hz, 2H), 1.19 (s, 9H), 1.15 (t, J=7.2 Hz, 3H).

المصدر