반응 #582637

ord-a6595046bb5b4d8dbbd4426b89f2d4ff

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척the mixture was washed twice with 1M HCl, twice with 1M NaOH, water and brine
  2. 2
    기타Removal of the solvent under reduced pressure

실험 절차

2-(2-Methoxy-5-nitrophenyl)acetic acid (17.1 g, 1 eq, Step B), EDC (18.6 g, 1.2 eq.), Et3N (9.8 g, 13.6 mL, 1.2 eq) and dimethylamine hydrochloride (7.9 g, 1.2 eq.) in 150 mL of CH2Cl2 were stirred together with exclusion of air overnight. CH2Cl2 (150 mL) was added and the mixture was washed twice with 1M HCl, twice with 1M NaOH, water and brine. Removal of the solvent under reduced pressure followed by silica gel chromatography (90:10 CH2Cl2:EtOAc) afforded pure 2-(2-methoxy-5-nitrophenyl)-N,N-dimethyl-acetamide as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06939874B2uspto-grants-2005_09