2,6-Dimethylaniline → N-(2,6-dimethylphenyl)-2-methoxyacetamide

HRID 1156833ノート

反応式

HRID 1156833 の反応式
[CH3:1][O:2][CH2:3][C:4](Cl)=[O:5].[CH3:7][C:8]1[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[C:9]=1[NH2:10].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:7][C:8]1[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[C:9]=1[NH:10][C:4](=[O:5])[CH2:3][O:2][CH3:1]

参加物

5

反応物 3

HCID 68962,6-DimethylanilineHCID 8471TriethylamineHCID 96623Methoxyacetyl chloride

生成物 1

HCID 10878014N-(2,6-dimethylphenyl)-2-methoxyacetamide収率 57%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

55 g (0.5 mol) of methoxyacetyl chloride were added dropwise to a solution of 61 g (0.5 mol) of 2,6-dimethylaniline and 50.5 g (0.5 mol) of triethylamine in 250 ml of toluene at 5° to 15° C., while stirring and cooling. The mixture was subsequently stirred at 20° C. for 2 hours, filtered and concentrated and the residue was taken up in water. The aqueous mixture was extracted with methylene chloride and the extract was dried over sodium sulphate and concentrated by distilling off the solvent. The residue was distilled under a high vacuum. 55 g (57% of theory) of 2,6-dimethyl-N-methoxyacetyl-aniline of boiling point 122°-132° C./0.1 mm Hg and of melting point 61°-63° C. were obtained. ##STR177##

後処理

  1. temperaturecooling
  2. stirringThe mixture was subsequently stirred at 20° C. for 2 hours
  3. filtrationfiltered
  4. concentrationconcentrated
  5. extractionThe aqueous mixture was extracted with methylene chloride
  6. dry with materialthe extract was dried over sodium sulphate
  7. concentrationconcentrated
  8. distillationby distilling off the solvent
  9. distillationThe residue was distilled under a high vacuum

出典と根拠

ORDレコード
ord-8637958b54ba4c4181c22cb21766b6b4
出典データセット
uspto-grants-1982_06
特許番号
US04337268

反応ノート

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