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

HRID 249499노트

반응식

HRID 249499 반응식
[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

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 64246602-Bromo-5-bromomethylpyridine

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1d04b79853934d4391034ffc123dd4a3
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05214152

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