반응 #2364

반응 방정식

Compound A

N-{6-(2-aminoethoxy)-5-(3-methoxyphenoxy)pyrimidin-4-yl}-4-tert-butylbenzenesulfonamide hydrochloride

2-chloropyrimidine

potassium carbonate

dimethylacetamide

→

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

수율 161.1%

용매

ammonium chloride

반응 조건

후처리

1. 1
   온도is heated
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The extract is washed
4. 4
   기타dried
5. 5
   기타The solvent is evaporated
6. 6
   기타to remove the solvent
7. 7
   기타the residue is purified by silica gel column chromatography (solvent; chloroform/methanol=100:1)
8. 8
   기타further recrystallized from ethyl acetate/n-hexane

실험 절차

A mixture of Compound A (150 mg), 2-chloropyrimidine (61 mg), potassium carbonate (122 mg) and dimethylacetamide (1.5 ml) is heated with stirring at 100° C. for three days. The reaction solution is diluted with aqueous ammonium chloride solution, and extracted with ethyl acetate. The extract is washed and dried. The solvent is evaporated to remove the solvent, and the residue is purified by silica gel column chromatography (solvent; chloroform/methanol=100:1) and further recrystallized from ethyl acetate/n-hexane to give 4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(2-pyrimidinylamino)ethoxy}-pyrimidin-4-yl]benzenesulfonamide hydrate (135 mg) as crystals.

출처