تفاعل #2074048

معادلة التفاعل

4-{[4-(tert-butoxycarbonylamino-methyl)-cyclohexylmethyl]-amino}-2-(2-chloro-benzylamino)-pyrimidine-5-carboxylic acid

EtOH

HCl dioxane

→

title compound

المردود 52.9%

4-[(4-aminomethyl-cyclohexylmethyl)-amino]-2-(2-chloro-benzylamino)-pyrimidine-5-carboxylic acid

المردود 52.9%

المذيبات

CHCl3

ظروف التفاعل

المعالجة

1. 1
   تركيزthen concentrated in vacuo
2. 2
   أخرىto provide a crude white powder
3. 3
   أخرىThe crude material was purified by preparative scale reverse phase HPLC
4. 4
   تركيزconcentrated in vacuo

الإجراء التجريبي

To a solution of 4-{[4-(tert-butoxycarbonylamino-methyl)-cyclohexylmethyl]-amino}-2-(2-chloro-benzylamino)-pyrimidine-5-carboxylic acid (80 mg, 0.159 mmol) dissolved in 2:1 CHCl3:EtOH at room temperature was added 4.0 M HCl/dioxane (5.0 mL). The mixture was stirred at room temperature for 2 h then concentrated in vacuo to provide a crude white powder. The crude material was purified by preparative scale reverse phase HPLC using a 0.1% TFA-H2O/CH3CN mobile phase. The product-containing fractions were combined and concentrated in vacuo to provide 34 mg of the title compound as a white solid, 53%, m/z calculated for C20H26ClN5O2: 403.9, found: 404.4 (M+H)+.

المصدر