تفاعل #2342475

معادلة التفاعل

dimethylaminopyridine

4-Aminobenzamidine di-HCl

DMF

succinic anhydride

→

4-[[4-(aminoiminomethyl)phenyl]amino]-4-oxo-butanoic acid

المردود 88.0%

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwere added
2. 2
   أخرىThe product precipitated 20
3. 3
   ترشيحThe product was filtered
4. 4
   غسيلwashed with water, acetonitrile and ether
5. 5
   workup.ADDITION4N HCl in dioxane (100 ml) was added
6. 6
   ترشيحfiltered
7. 7
   أخرىdried in a desiccator

الإجراء التجريبي

4-Aminobenzamidine di-HCl (25 g, 120 mmol), which is commercially available particularly from Aldrich, was added to dry DMF (100 ml). To this solution dry pyridine (100 ml) and succinic anhydride (12 g, 120 mmol) followed by dimethylaminopyridine (DMAP 1.5 g 0.012 mmol) were added. The product precipitated 20 after heating for 1/2h at 100° C. The product was filtered, washed with water, acetonitrile and ether. The light solid was suspended in dioxane, 4N HCl in dioxane (100 ml) was added and the suspension was stirred for 1 h, filtered and dried in a desiccator to give 28 g, 88% of 4-[[4-(aminoiminomethyl)phenyl]amino]-4-oxo-butanoic acid as a white yellow solid which decomposes between 270° and 290° C.

المصدر