Reaktion #4438

ord-917a2479c3f9457d87255a214f0059bb

Reaktionsgleichung

ClC(Cl)Cl
chloroform
COc1ccc(-c2cc(Nc3ccc(N)cc3)nc(C)n2)cc1OC
4-(4-aminophenylamino)-6-(3,4-dimethoxyphenyl)-2-methylpyrimidine
CS(=O)(=O)Cl
methanesulfonyl chloride
CCN(CC)CC
triethylamine
COc1ccc(-c2cc(Nc3ccc(NS(C)(=O)=O)cc3)nc(C)n2)cc1OC
6-(3,4-dimethoxyphenyl)-4-(4-mesylaminophenylamino)-2-methylpyrimidine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was refluxed for 3 hours
  2. 2
    TemperaturAfter cooled
  3. 3
    Waschenwashed with water
  4. 4
    TrocknenThe solution was dried over magnesium sulfate
  5. 5
    Sonstigeevaporated
  6. 6
    Sonstigechromatographed on silica gel eluting with chloroform

Vorschrift

To a solution of 4-(4-aminophenylamino)-6-(3,4-dimethoxyphenyl)-2-methylpyrimidine (1.0 g) in 1,2-dichloroethane (20 ml) were added methanesulfonyl chloride (0.28 ml) and triethylamine (0.83 ml) and the mixture was refluxed for 3 hours. After cooled, chloroform (50 ml) was added thereto, and washed with water. The solution was dried over magnesium sulfate, evaporated, and chromatographed on silica gel eluting with chloroform to give 6-(3,4-dimethoxyphenyl)-4-(4-mesylaminophenylamino)-2-methylpyrimidine (0.45 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04725600uspto-grants-1988_02