تفاعل #809592

معادلة التفاعل

HCl

N-(4-fluoro-3-nitro-phenyl)-N-methyl-benzamide

DIEA

β-alanine amide hydrochloride

→

N-[4-(2-carbamoyl-ethylamino)-3-nitro-phenyl]-N-methyl-benzamide

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe aqueous layer was extracted 3× with ethyl acetate
2. 2
   غسيلThe combined organic layers were washed with water, brine
3. 3
   تجفيفdried over magnesium sulfate
4. 4
   ترشيحThe solution was filtered
5. 5
   أخرىthe solvent removed under reduced pressure
6. 6
   أخرىThe residue was triturated twice with cold hexane
7. 7
   أخرىdried

الإجراء التجريبي

N-(4-fluoro-3-nitro-phenyl)-N-methyl-benzamide (1.47 g, 5.37 mmol) was taken up in dry acetonitrile under argon, DIEA (2.08 g, 16.11 mmol, 2.80 ml) and β-alanine amide hydrochloride (1.00 g, 8.06 mmol) were added. The reaction mixture was heated to 80° C. for 48 h. The reaction was poured into 1N HCl and the aqueous layer was extracted 3× with ethyl acetate. The combined organic layers were washed with water, brine and dried over magnesium sulfate. The solution was filtered and the solvent removed under reduced pressure. The residue was triturated twice with cold hexane and dried to give N-[4-(2-carbamoyl-ethylamino)-3-nitro-phenyl]-N-methyl-benzamide. (1.75 g, 95%)

المصدر