تفاعل #48605

معادلة التفاعل

4-{[4-(2,6-dichloro-benzoylamino)-1H-pyrazole-3-carbonyl]-amino}-piperidine-1-carboxylic acid tert-butyl ester

HCl EtOAc

→

4-(2,6-dichloro-benzoylamino)-1H-pyrazole-3-carboxylic acid piperidin-4-ylamide

المردود 100.6%

المذيبات

MeOH

EtOAc

ظروف التفاعل

المعالجة

1. 1
   أخرىThe product did not crystallise due to the presence of methanol
2. 2
   أخرىthe reaction mixture was evaporated
3. 3
   أخرىthe residue triturated with EtOAc
4. 4
   ترشيحThe resulting off white solid was collected by filtration
5. 5
   غسيلwashed with EtOAc
6. 6
   أخرىsucked dry on the sinter

الإجراء التجريبي

A solution of 4-{[4-(2,6-dichloro-benzoylamino)-1H-pyrazole-3-carbonyl]-amino}-piperidine-1-carboxylic acid tert-butyl ester (7.9 g) in MeOH (50 mL) and EtOAc (50 ml) was treated with sat. HCl-EtOAc (40 mL) then stirred at r.t. overnight. The product did not crystallise due to the presence of methanol, and therefore the reaction mixture was evaporated and the residue triturated with EtOAc. The resulting off white solid was collected by filtration, washed with EtOAc and sucked dry on the sinter to give 6.3 g of 4-(2,6-dichloro-benzoylamino)-1H-pyrazole-3-carboxylic acid piperidin-4-ylamide as the hydrochloride salt. (LC/MS: Rt 5.89, [M+H]+ 382/384).

المصدر