반응 #166409

반응 방정식

chloroacetyl chloride

compound 397

4-(aminomethyl)-1-benzylpiperidin-4-ol

triethylamine

→

compound 398

수율 78.4%

N-((1-benzyl-4-hydroxypiperidin-4-yl)methyl)-2-chloroacetamide

수율 78.4%

용매

DCM

water

dichloromethane

반응 조건

후처리

1. 1
   추출extracted with DCM twice
2. 2
   건조The combined organics were dried over Na2SO4
3. 3
   농축concentrated in vacuo

실험 절차

To a solution of compound 397 (39.7 g, 180 mmol) in dichloromethane (350 mL) was added triethylamine (50.0 mL, 359 mmol), followed by dropwise addition of chloroacetyl chloride (16.5 mL, 207 mmol) over 15 minutes. The resulting solution was stirred at room temperature for 1.25 hours. The crude mixture was diluted with DCM and water, and extracted with DCM twice. The combined organics were dried over Na2SO4 and concentrated in vacuo to give compound 398 (41.9 g, 78%). LCMS-ESI (POS), M/Z, M+1: Found 297.1, Calculated 297.1.

출처