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

HRID 1585017노트

반응식

HRID 1585017 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8ae098a604d143a295e512ff516dc255
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05935981

반응 노트

불러오는 중…