Reaktion #2362

Reaktionsgleichung

ammonium chloride

4-tert-butyl-N-{6-chloro-5-(3-methoxyphenoxy)pyrimidin-4-yl}benzenesulfonamide

pyridine-2-methanol

sodium hydride

→

4-tert-butyl-N-{5-(3-methoxyphenoxy)-6-(2-pyridinylmethoxy)pyrimidin-4-yl}benzenesulfonamide

Ausbeute 94.6%

Lösungsmittel

dimethylacetamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling
2. 2
   SonstigeThe mixture is reacted at 100° C. for 30 minutes
3. 3
   Temperaturcooled
4. 4
   ExtraktionThe mixture is extracted with ethyl acetate
5. 5
   Waschenthe extract is washed
6. 6
   Sonstigedried
7. 7
   Einengenconcentrated to dryness under reduced pressure
8. 8
   SonstigeThe residue is crystallized from ethyl acetate

Vorschrift

To a stirred solution of pyridine-2-methanol (130 mg) in dimethylacetamide (0.5 ml) is added gradually with stirring sodium hydride (62.7% dispersion-type, 60 mg) under ice-cooling, and thereto is added 4-tert-butyl-N-{6-chloro-5-(3-methoxyphenoxy)pyrimidin-4-yl}benzenesulfonamide (100 mg). The mixture is reacted at 100° C. for 30 minutes, and cooled. The pH value of the mixture is adjusted to pH 8 with saturated aqueous ammonium chloride solution. The mixture is extracted with ethyl acetate, and the extract is washed, dried, and concentrated to dryness under reduced pressure. The residue is crystallized from ethyl acetate to give 4-tert-butyl-N-{5-(3-methoxyphenoxy)-6-(2-pyridinylmethoxy)pyrimidin-4-yl}benzenesulfonamide (110 mg) as crystals.

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