Methylamine → 6-(2-Chlorophenyl)-5-(4-chlorophenyl)-2-(methylamino)pyridine-3-carbonitrile

HRID 13815노트

반응식

HRID 13815 반응식
Cl[C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)=[C:4]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[N:3]=1.[NH2:24][CH3:25]>>[Cl:23][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[C:4]1[N:3]=[C:2]([NH:24][CH3:25])[C:7]([C:8]#[N:9])=[CH:6][C:5]=1[C:10]1[CH:11]=[CH:12][C:13]([Cl:16])=[CH:14][CH:15]=1

참가 물질

3

반응물 2

HCID 6329MethylamineHCID 102371012-Chloro-6-(2-chlorophenyl)-5-(4-chlorophenyl)nicotinonitrile

생성물 1

HCID 687190996-(2-Chlorophenyl)-5-(4-chlorophenyl)-2-(methylamino)pyridine-3-carbonitrile

실험 절차

To the product of Step C (300 mg) was added H2NCH3 (3.34 mL, 2 M solution in THF). The reaction stirred at room temperature overnight 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 20% EtOAc in hexane affording the title compound. HPLC/MS: 353.9 (M+1), 355.9 (M+3); Rt=4.21 min.

후처리

  1. concentrationbefore concentrating
  2. dissolutionThe product was dissolved in EtOAc
  3. washwashed with saturated aqueous NaHCO3 solution
  4. concentrationThe solution was concentrated
  5. custompurified via flash chromatography on silica gel with a gradient elution of 0% to 20% EtOAc in hexane affording the title compound

출처 및 근거

ORD 기록
ord-6580fa0bfeac4e7fad3eaafdcf660b82
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728141B2

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