반응 #710545

반응 방정식

NaHCO3

(4-fluoro-phenyl)-isobutyl-amine

5-bromo-pyridine-2-sulfonyl chloride

pyridine

→

5-bromo-pyridine-2-sulfonic acid (4-fluoro-phenyl)-isobutyl-amide

수율 82.9%

용매

Water

DCM

DCM

반응 조건

후처리

1. 1
   추출extracted with DCM
2. 2
   여과filtered through a phase separator
3. 3
   농축concentrated
4. 4
   기타then purified by silica gel column chromatography (0-20% EtOAc in cyclohexane)

실험 절차

To a solution of 5-bromo-pyridine-2-sulfonyl chloride (330 mg, 1.29 mmol) in DCM (10 mL) was added pyridine (208 μL, 2.57 mmol) followed by a solution of (4-fluoro-phenyl)-isobutyl-amine (215 mg, 1.29 mmol) in DCM (10 mL) and the reaction was stirred at room temperature for 16 hours. Water and saturated aqueous NaHCO3 were added and then extracted with DCM, filtered through a phase separator, concentrated then purified by silica gel column chromatography (0-20% EtOAc in cyclohexane) to give 5-bromo-pyridine-2-sulfonic acid (4-fluoro-phenyl)-isobutyl-amide (414 mg, 78%). LCMS (m/z, Method A) ES+ 387/389 [M+1]+.

출처