Methylamine → 6-Bromo-N-methyl-3-pyridinemethanamine

HRID 249499ノート

反応式

HRID 249499 の反応式
[CH3:1][NH2:2].[Br:3][C:4]1[N:9]=[CH:8][C:7]([CH2:10]Br)=[CH:6][CH:5]=1>CC#N>[Br:3][C:4]1[N:9]=[CH:8][C:7]([CH2:10][NH:2][CH3:1])=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 64246602-Bromo-5-bromomethylpyridine

生成物 1

HCID 224503166-Bromo-N-methyl-3-pyridinemethanamine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a mixture of 12.3 g of 40% aqueous methylamine solution and 40 ml of CH3CN was added 8.0 g of crude (6-bromo-3-pyridyl)methyl bromide with stirring. The mixture was further stirred at room temperature for 30 minutes. The reaction mixture thus obtained was concentrated and the residue was diluted with toluene and subjected to azeotropic distillation to remove the water. Then, the soluble fraction was extracted with Et2O. The Et2O layer was dried over MgSO4 and concentrated to recover 4.4 g of the title compound as a yellow oil.

後処理

  1. stirringThe mixture was further stirred at room temperature for 30 minutes
  2. customThe reaction mixture thus obtained
  3. concentrationwas concentrated
  4. additionthe residue was diluted with toluene
  5. distillationsubjected to azeotropic distillation
  6. customto remove the water
  7. extractionThen, the soluble fraction was extracted with Et2O
  8. dry with materialThe Et2O layer was dried over MgSO4
  9. concentrationconcentrated
  10. customto recover 4.4 g of the title compound as a yellow oil

出典と根拠

ORDレコード
ord-1d04b79853934d4391034ffc123dd4a3
出典データセット
uspto-grants-1993_05
特許番号
US05214152

反応ノート

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