Methylamine → 2-Methyl-5-[(methylamino)methyl]pyridine

HRID 1585017ノート

反応式

HRID 1585017 の反応式
[CH3:1][NH2:2].[CH3:3][C:4]1[N:9]=[CH:8][C:7]([CH2:10]Cl)=[CH:6][CH:5]=1>CC#N>[CH3:1][NH:2][CH2:10][C:7]1[CH:8]=[N:9][C:4]([CH3:3])=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 122143385-(Chloromethyl)-2-methylpyridine

生成物 1

HCID 154773072-Methyl-5-[(methylamino)methyl]pyridine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 16.6 g of 40% aqueous MeNH2 solution and 52 ml of CH3CN was cooled with ice and 6.08 g (0.043 mole in terms of pure product) of crude (6-methyl-3-pyridyl)-methyl chloride was added dropwise with constant stirring. After completion of dropwise addition, the mixture was stirred at room temperature for 1.5 hours, at the end of which time the solvent was distilled off. The solid residue was extracted with CH2Cl2 and the CH2Cl2 layer was dried over MgSO4. The CH2Cl2 was distilled off and the residue was diluted with 70 ml of Et2O and filtered to remove the insoluble matter. Finally the filtrate was concentrated to recover 4.60 g of the title compound as a crude oil.

後処理

  1. additionwas added dropwise with constant stirring
  2. additionAfter completion of dropwise addition
  3. distillationwas distilled off
  4. extractionThe solid residue was extracted with CH2Cl2
  5. dry with materialthe CH2Cl2 layer was dried over MgSO4
  6. distillationThe CH2Cl2 was distilled off
  7. additionthe residue was diluted with 70 ml of Et2O
  8. filtrationfiltered
  9. customto remove the insoluble matter
  10. concentrationFinally the filtrate was concentrated
  11. customto recover 4.60 g of the title compound as a crude oil

出典と根拠

ORDレコード
ord-8ae098a604d143a295e512ff516dc255
出典データセット
uspto-grants-1999_08
特許番号
US05935981

反応ノート

読み込み中…