Triethylamine → N-Formylmethyl-3-methoxy-N-(2-methoxyphenyl)benzamide

HRID 2464

反応式

HRID 2464 の反応式
[OH:1][CH2:2][CH2:3][N:4]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[O:21][CH3:22])[C:5](=[O:14])[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH3:13])[CH:7]=1.C(N(CC)CC)C>CS(C)=O>[CH:2]([CH2:3][N:4]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[O:21][CH3:22])[C:5](=[O:14])[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH3:13])[CH:7]=1)=[O:1]

参加物

4

反応物 2

HCID 8471TriethylamineHCID 19689855N-(2-hydroxyethyl)-3-methoxy-N-(2-methoxyphenyl)benzamide

生成物 1

HCID 19689822N-Formylmethyl-3-methoxy-N-(2-methoxyphenyl)benzamide収率 65.6%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

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.

後処理

  1. customat room temperature
  2. extractionextracted with ethyl acetate
  3. washwashed with water and saturated brine
  4. dry with materialThe resulting organic layer was dried on anhydrous magnesium sulfate
  5. customthe solvent was removed by evaporation

出典と根拠

ORDレコード
ord-18e129f85987443abf273cc4ec32d571
出典データセット
uspto-grants-1998_03
特許番号
US05728835

関連ノート

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