تفاعل #2397

معادلة التفاعل

hydrochloric acid

1,3-propanediol

sodium hydride

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

→

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

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction mixture is reacted at 90° C. for two hours
2. 2
   أخرىreacted at 130° C. for one hour
3. 3
   استخلاصextracted with ethyl acetate
4. 4
   غسيلthe ethyl acetate layer is washed
5. 5
   أخرىdried
6. 6
   تركيزconcentrated to dryness under reduced pressure
7. 7
   أخرىThe residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=10:1)
8. 8
   أخرىcrystallized from ethyl acetate/diisopropyl ether

الإجراء التجريبي

To 1,3-propanediol (7 ml) is added sodium hydride (60% dispersion-type, 312 mg), and thereto is added 4-tert-butyl-N-{6-chloro-5-(3-methoxyphenoxy)pyrimidin-4-yl}benzenesulfonamide (707 mg). The reaction mixture is reacted at 90° C. for two hours, and then reacted at 130° C. for one hour. The reaction solution is acidified with 10% hydrochloric acid, and extracted with ethyl acetate, and the ethyl acetate layer is washed, dried, and concentrated to dryness under reduced pressure. The residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=10:1), and crystallized from ethyl acetate/diisopropyl ether to give 4-tert-butyl-N-{6-(3-hydroxypropyloxy)-5-(3-methoxyphenoxy)pyrimidin-4-yl}benzenesulfonamide (315 mg) as crystals.

المصدر