反応 #1922792

反応方程式

Succinimidyl nicotinate

3-amino-3-(N-(6-(4,6-diphenyl(2-pyridyloxy))-2,2-dimethylhexyl)carbamoyl)propanoic acid

N,N-dimethylformamide

triethylamine

→

3-(N-(6-(4,6-diphenyl(2-pyridyloxy))-2,2-dimethylhexyl)carbamoyl)-3-(3-pyridylcarbonylamino)propanoic acid

溶媒

acetonitrile water

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred for 18 h
2. 2
   濃縮The mixture was concentrated under high vacuum
3. 3
   その他the residue was purified
4. 4
   workup.ADDITIONreverse-phase HPLC (water-acetonitrile gradient containing 0.1% TFA)
5. 5
   その他to afford 23 mg (19%) of

実験手順

A mixture of 3-amino-3-(N-(6-(4,6-diphenyl(2-pyridyloxy))-2,2-dimethylhexyl)carbamoyl)propanoic acid (100 mg, 0.204 mmol), N,N-dimethylformamide (2 mL), and triethylamine (0.1 mL) was stirred at room temperature for 5 min. Succinimidyl nicotinate (69 mg, 0.315 mmol) was added, and the mixture was stirred for 18 h. The mixture was concentrated under high vacuum, and the residue was purified using reverse-phase HPLC (water-acetonitrile gradient containing 0.1% TFA) to afford 23 mg (19%) of a white powdered solid. ESMS: Calculated for C35H38N4O5, 594.2842 Found 595.2 [M+H]+1; Rt=15.597 min (100% pure, Vydac C18 column; gradient 20 to 100% acetonitrile/water+0.1% TFA over 30 min).

出典