تفاعل #435800

معادلة التفاعل

compound

4-(4-{[bis-(1H-imidazol-2-ylmethyl)-amino]-methyl}-benzoyl)-piperazin-1-carboxylic acid t-butyl ester

hydrogen chloride dioxane

→

compound

المردود 55.2%

(4-{[bis-(1H-imidazol-2-ylmethyl)-amino]-methyl}-phenyl)-piperazin-1-yl-methanone

المردود 55.2%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter completion of the reaction
2. 2
   workup.DISTILLATIONthe solvent was distilled off
3. 3
   workup.ADDITIONthe residue was added with a 1 mol/l sodium hydroxide aqueous solution
4. 4
   غسيلby washing with dichloromethane
5. 5
   أخرىThe aqueous layer was evaporated to dryness
6. 6
   workup.DISTILLATIONby distilling azeotropically with chloroform

الإجراء التجريبي

The compound (111 mg) obtained in Example 32-1 was dissolved in anhydrous methanol (1.0 ml) and then added with a 4 mol/l hydrogen chloride/dioxane solution (3.0 ml) and stirred at room temperature for 1 hour. After completion of the reaction, the solvent was distilled off and the residue was added with a 1 mol/l sodium hydroxide aqueous solution, followed by washing with dichloromethane. The aqueous layer was evaporated to dryness, followed by distilling azeotropically with chloroform. Consequently, the subject compound (48.5 mg) was obtained as a yellow oily substance.

المصدر