تفاعل #1998026

معادلة التفاعل

1-(4-methoxybenzyl)-1H-pyrazole-4-carboxamide

Lawesson's reagent

→

1-(4-methoxybenzyl)-1H-pyrazole-4-carbothioamide

المردود 51.2%

المذيبات

CHCl3 toluene

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction mixture was evaporated
2. 2
   أخرىthe residue was recrystallized in EtOAc/pentane

الإجراء التجريبي

According to Scheme 1 Step 4: A solution of 1-(4-methoxybenzyl)-1H-pyrazole-4-carboxamide (109 mmol, 25.1 g) and Lawesson's reagent (109 mmol, 43.9 g) in CHCl3/toluene (1:1, 136 mL) was stirred at 85° C. for 12 hours. The reaction mixture was evaporated and the residue was recrystallized in EtOAc/pentane to yield 13.8 g of 1-(4-methoxybenzyl)-1H-pyrazole-4-carbothioamide. The mother liquors were evaporated and the crude residue was purified by flash chromatography over silica gel using DCM/EtOAc (100:0 to 70:30) to yield 1-(4-methoxybenzyl)-1H-pyrazole-4-carbothioamide (94.6 mmol, 23.4 g, 87%) as a beige solid.

المصدر