تفاعل #462458

معادلة التفاعل

water

N-tert-butyl-2-[3-bromo-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H-(1)benzazepin-1-yl] ethanoic acid amide

dimethylformamide

sodium azide

→

N-tert-butyl-2-[3-azido-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H-(1)benzazepin-1-yl] ethanoic acid amide

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   أخرىTo a 250 ml round-bottomed flask equipped with N2 inlet
2. 2
   درجة الحرارةThe reaction mixture was then cooled
3. 3
   أخرىseparated
4. 4
   استخلاصthe aqueous phase was again extracted
5. 5
   غسيلThe combined extracts were washed with water three times, with bicarbonate solution once
6. 6
   تجفيفdried with brine and sodium sulfate
7. 7
   ترشيحfiltered
8. 8
   أخرىevaporated
9. 9
   أخرىleaving a gummy residue, 8.58 g (100%)
10. 10
    workup.ADDITIONcontaining some solvent

الإجراء التجريبي

To a 250 ml round-bottomed flask equipped with N2 inlet were added N-tert-butyl-2-[3-bromo-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H-(1)benzazepin-1-yl] ethanoic acid amide, (8.317 g, 19.37 mmoles), 90 ml dimethylformamide (DMF), and sodium azide (5.25 g, 80 mmoles, under nitrogen), and the mixture was heated at 75° C. for 20 hours with stirring. The reaction mixture was then cooled and distributed between water and ethyl acetate, separated, and the aqueous phase was again extracted. The combined extracts were washed with water three times, with bicarbonate solution once, and then dried with brine and sodium sulfate and filtered and evaporated, leaving a gummy residue, 8.58 g (100%), containing some solvent.

المصدر