반응 #2560

ord-18e129f85987443abf273cc4ec32d571

반응 방정식

COc1cccc(C(=O)N(CCO)c2ccccc2OC)c1
N-(2-hydroxyethyl)-3-methoxy-N-(2-methoxyphenyl)benzamide
CCN(CC)CC
triethylamine
COc1cccc(C(=O)N(CC=O)c2ccccc2OC)c1
title compound
수율 65.6%
COc1cccc(C(=O)N(CC=O)c2ccccc2OC)c1
N-Formylmethyl-3-methoxy-N-(2-methoxyphenyl)benzamide
수율 65.6%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at room temperature
  2. 2
    추출extracted with ethyl acetate
  3. 3
    세척washed with water and saturated brine
  4. 4
    건조The resulting organic layer was dried on anhydrous magnesium sulfate
  5. 5
    기타the solvent was removed by evaporation

실험 절차

In an atmosphere of argon, N-(2-hydroxyethyl)-3-methoxy-N-(2-methoxyphenyl)benzamide (339 mg, 1.12 mmol) was dissolved in DMSO (4 ml) to which were subsequently added dropwise triethylamine (0.724 ml, 5.20 mmol) and a DMSO solution (8 ml) of a sulfur trioxide-pyridine complex (844 mg, 5.20 mmol) at room temperature. After 20 minutes of stirring at the same temperature, this was mixed with ice water (40 ml) and extracted with ethyl acetate, and then washed with water and saturated brine. The resulting organic layer was dried on anhydrous magnesium sulfate, and the solvent was removed by evaporation to obtain 220 mg (65.6%) of the title compound the form of light yellow solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728835uspto-grants-1998_03