반응 #1113

ord-81b10c28bd9c47d5984b354d59da9d19

반응 방정식

[Cl-].[NH4+]
ammonium chloride
[H-].[Na+]
NaH
COc1c(Cl)ccnc1C
2-methyl-3-methoxy-4-chloropyridine
CC(C)(C)c1ccc(OCCO)cc1
2-(4-tert-butylphenoxy)ethanol
COc1c(OCCOc2ccc(C(C)(C)C)cc2)ccnc1C
2-Methyl-3-methoxy-4-[2-(4-tert-butylphenoxy)ethoxy]pyridine

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the mixture is extracted with ethyl acetate
  2. 2
    기타The reaction product is purified by chromatography (SiO2 ; EtOAc)

실험 절차

A mixture of 1.57 g (10 mmol) of 2-methyl-3-methoxy-4-chloropyridine, 2.52 g (13 mmol) of 2-(4-tert-butylphenoxy)ethanol and 15 ml of DMSO is added dropwise at 25° C. to 0.36 g (12 mmol) of NaH (80% strength) in 25 ml of DMSO. The mixture is then stirred at 60° C. for 5 hours. For working up, saturated ammonium chloride solution is added at 20° to 25° C. and the mixture is extracted with ethyl acetate. The reaction product is purified by chromatography (SiO2 ; EtOAc). Yield: 2.63 g (74.9%); m.p.: 84° to 87° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723450uspto-grants-1998_03