Methylamine → 5-Bromo-2-ethoxy-N,4-dimethylbenzamide

HRID 1295922ノート

反応式

HRID 1295922 の反応式
[Br:1][C:2]1[C:3]([CH3:14])=[CH:4][C:5]([O:11][CH2:12][CH3:13])=[C:6]([CH:10]=1)[C:7](O)=[O:8].[CH3:15][NH2:16].C(OCC)(=O)C>O1CCCC1.C(N(CC)CC)C.ClC(OCC)=O>[CH3:15][NH:16][C:7](=[O:8])[C:6]1[CH:10]=[C:2]([Br:1])[C:3]([CH3:14])=[CH:4][C:5]=1[O:11][CH2:12][CH3:13]

参加物

7

反応物 3

HCID 6329MethylamineHCID 8857Ethyl AcetateHCID 22929762HCID 22929762、化合物

生成物 1

HCID 229298455-Bromo-2-ethoxy-N,4-dimethylbenzamide

試薬・触媒・溶媒 3

HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒HCID 10928Ethyl chloroformate溶媒

実験手順

After dissolving 5-bromo-2-ethoxy-4-methylbenzoic acid in tetrahydrofuran (80 ml), triethylamine (3.5 ml) and ethyl chloroformate (2.4 ml) were added while cooling on ice, the mixture was stirred for 1 hour, and then a 40% methylamine aqueous solution (3.5 ml) was added. The reaction mixture was stirred for 1 hour, ethyl acetate was added and the mixture was washed with brine, after which the organic layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The crystals of the residue were washed with hexane and filtered to yield the title compound (5.08 g) as white crystals.

後処理

  1. additionwere added
  2. temperaturewhile cooling on ice
  3. stirringThe reaction mixture was stirred for 1 hour
  4. washthe mixture was washed with brine
  5. dry with materialafter which the organic layer was dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. washThe crystals of the residue were washed with hexane
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-5de0f3fe9e4c45a9924d44fcaebdefbe
出典データセット
uspto-grants-2007_07
特許番号
US07244730B2

反応ノート

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