반응 #42080

반응 방정식

2-chloro-6-(2,4-dichlorophenyl)-5-(4-chlorophenyl)pyridine-3-carbonitrile

H2NCH3

→

6-(2,4-dichlorophenyl)-5-(4-chlorophenyl)-2-(methylamino)pyridine-3-carbonitrile

용매

THF

반응 조건

후처리

1. 1
   농축before concentrating
2. 2
   workup.DISSOLUTIONThe product was dissolved in EtOAc
3. 3
   세척washed with saturated aqueous NaHCO3 solution
4. 4
   농축The solution was concentrated
5. 5
   기타purified via flash chromatography on silica gel with a gradient elution of 0% to 10% EtOAc in hexane affording the title compound

실험 절차

To 2-chloro-6-(2,4-dichlorophenyl)-5-(4-chlorophenyl)pyridine-3-carbonitrile (2.03 g) in THF (14 mL) was added H2NCH3 (13 mL, 2 M solution in THF). The reaction was heated to 67° C. in a closed vessel for 9 hours before concentrating. The product was dissolved in EtOAc and washed with saturated aqueous NaHCO3 solution. The solution was concentrated and purified via flash chromatography on silica gel with a gradient elution of 0% to 10% EtOAc in hexane affording the title compound. HPLC/MS: 387.8(M+1), 389.8 (M+3); Rt=4.26 min.

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