2-Aminopropanol → 1-Methyl-2-(4-pyridyloxy)ethylamine

HRID 1900168

反応式

HRID 1900168 の反応式
[NH2:1][CH:2]([CH3:5])[CH2:3][OH:4].[H-].[Na+].Cl.Cl[C:10]1[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=1>CN(C)C=O>[CH3:5][CH:2]([NH2:1])[CH2:3][O:4][C:10]1[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=1

参加物

5

実験手順

6.2 g of 2-amino-1-propanol was added dropwise to a stirred mixture of 4.0 g of 60% sodium hydride and 50 mL of N,N-dimethylformamide at 5° C.-10° C. After the reaction mixture was stirred for 30 minutes, 12.5 g of 4-chloropyridine hydrochloride in limited amounts was added to the reaction mixture. The mixture was stirred for 20 hours at room temperature. After completion of the reaction, the solids were filtered off. The solvent in the filtrate was removed under reduced pressure. The residue was purified by column chromatography on silica gel to obtain 3.8 g of the desired product (yield: 30%). Refractive index: 1.5469.

後処理

  1. stirringThe mixture was stirred for 20 hours at room temperature
  2. customAfter completion of the reaction
  3. filtrationthe solids were filtered off
  4. customThe solvent in the filtrate was removed under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-64e63c4358cb4c6fbafa06e0eafb27bc
出典データセット
uspto-grants-1996_11
特許番号
US05574064

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