反応 #2368

反応方程式

4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(2-methylthiopyrimidin-4-yloxy)ethoxy}pyrimidin-4-yl]benzenesulfonamide

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4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(pyrimidin-4-yloxy)ethoxy}pyrimidin-4-yl]benzenesulfonamide

収率 32.9%

溶媒

ethanol

反応条件

後処理

1. 1
   温度the mixture is refluxed for four hours
2. 2
   その他Raney-nickel is removed by filtration
3. 3
   洗浄washed with ethanol and acetic acid
4. 4
   濃縮The filtrate is concentrated under reduced pressure
5. 5
   抽出the residue is extracted with ethyl acetate
6. 6
   洗浄The ethyl acetate layer is washed
7. 7
   その他dried
8. 8
   その他evaporated
9. 9
   その他to remove the solvent
10. 10
    その他The residue is purified by silica gel column chromatography (solvent; chloroform/methanol=10:1)
11. 11
    その他recrystallized from ethyl acetate/n-hexane

実験手順

A mixture of 4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(2-methylthiopyrimidin-4-yloxy)ethoxy}pyrimidin-4-yl]benzenesulfonamide (250 mg), Raney-nickel (W-2) (2 g) and ethanol (5 ml) is stirred at room temperature overnight, and the mixture is refluxed for four hours. Raney-nickel is removed by filtration, and washed with ethanol and acetic acid. The filtrate is concentrated under reduced pressure, and the residue is extracted with ethyl acetate. The ethyl acetate layer is washed, dried, and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; chloroform/methanol=10:1), and recrystallized from ethyl acetate/n-hexane to give 4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(pyrimidin-4-yloxy)ethoxy}pyrimidin-4-yl]benzenesulfonamide (76 mg) as crystals.

出典