反応 #2362

反応方程式

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

収率 94.6%

溶媒

dimethylacetamide

反応条件

後処理

1. 1
   温度cooling
2. 2
   その他The mixture is reacted at 100° C. for 30 minutes
3. 3
   温度cooled
4. 4
   抽出The mixture is extracted with ethyl acetate
5. 5
   洗浄the extract is washed
6. 6
   その他dried
7. 7
   濃縮concentrated to dryness under reduced pressure
8. 8
   その他The residue is crystallized from ethyl acetate

実験手順

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.

出典