반응 #2362

반응 방정식

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

수율 94.6%

용매

dimethylacetamide

반응 조건

후처리

1. 1
   온도cooling
2. 2
   기타The mixture is reacted at 100° C. for 30 minutes
3. 3
   온도cooled
4. 4
   추출The mixture is extracted with ethyl acetate
5. 5
   세척the extract is washed
6. 6
   기타dried
7. 7
   농축concentrated to dryness under reduced pressure
8. 8
   기타The residue is crystallized from ethyl acetate

실험 절차

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.

출처