تفاعل #2368

معادلة التفاعل

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

المردود 32.9%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture is refluxed for four hours
2. 2
   أخرىRaney-nickel is removed by filtration
3. 3
   غسيلwashed with ethanol and acetic acid
4. 4
   تركيزThe filtrate is concentrated under reduced pressure
5. 5
   استخلاصthe residue is extracted with ethyl acetate
6. 6
   غسيلThe ethyl acetate layer is washed
7. 7
   أخرىdried
8. 8
   أخرىevaporated
9. 9
   أخرىto remove the solvent
10. 10
    أخرىThe residue is purified by silica gel column chromatography (solvent; chloroform/methanol=10:1)
11. 11
    أخرىrecrystallized from ethyl acetate/n-hexane

الإجراء التجريبي

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.

المصدر