تفاعل #2365

معادلة التفاعل

ammonium chloride

2-chloropyrimidine

Compound B

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

sodium hydride

→

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

المردود 92.5%

المذيبات

dimethylacetamide

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with ethyl acetate
2. 2
   غسيلThe ethyl acetate layer is washed
3. 3
   أخرىdried
4. 4
   أخرىevaporated
5. 5
   أخرىto remove the solvent
6. 6
   أخرىThe residue is purified by silica gel column chromatography (solvent; chloroform/methanol=20:1)
7. 7
   أخرىcrystallized from chloroform/diisopropyl ether

الإجراء التجريبي

To a solution of Compound B (116 mg) obtained in Example 19-(1) in dimethylacetamide (2 ml) is added sodium hydride (60% dispersion-type, 33 mg), and thereto is added 2-chloropyrimidine (40 mg). The reaction solution is stirred at room temperature overnight, and the mixture is treated with saturated aqueous ammonium chloride solution, and 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=20:1), and crystallized from chloroform/diisopropyl ether to give 4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(pyrimidin-2-yloxy)ethylamino}pyrimidin-4-yl]benzenesulfonamide (125 mg) as crystals.

المصدر