反应 #1023

ord-6d97a1bfa8604b93849d4516305a87c9

反应方程式

CC(N)CO
2-amino-1-propanol
[H-].[Na+]
sodium hydride
Cl.Clc1ccncc1
4-chloropyridine hydrochloride
CC(N)COc1ccncc1
desired product
收率 30.2%
CC(N)COc1ccncc1
1-methyl-2-(4-pyridyloxy)ethylamine
收率 30.2%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGThe mixture was stirred for 20 hours at room temperature
  2. 2
    其他After completion of the reaction
  3. 3
    过滤the solids were filtered off
  4. 4
    其他The solvent in the filtrate was removed under reduced pressure
  5. 5
    其他The residue was purified by column chromatography on silica gel

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723469uspto-grants-1998_03