반응 #1023

ord-6d97a1bfa8604b93849d4516305a87c9

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723469uspto-grants-1998_03