反応 #2560

ord-18e129f85987443abf273cc4ec32d571

反応方程式

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
収率 65.6%
COc1cccc(C(=O)N(CC=O)c2ccccc2OC)c1
N-Formylmethyl-3-methoxy-N-(2-methoxyphenyl)benzamide
収率 65.6%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他at room temperature
  2. 2
    抽出extracted with ethyl acetate
  3. 3
    洗浄washed with water and saturated brine
  4. 4
    乾燥The resulting organic layer was dried on anhydrous magnesium sulfate
  5. 5
    その他the solvent was removed by evaporation

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728835uspto-grants-1998_03