反应 #2560

ord-18e129f85987443abf273cc4ec32d571

反应方程式

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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他at room temperature
  2. 2
    萃取extracted with ethyl acetate
  3. 3
    洗涤washed with water and saturated brine
  4. 4
    干燥The resulting organic layer was dried on anhydrous magnesium sulfate
  5. 5
    其他the solvent was removed by evaporation

实验过程

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.

来源

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