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

참여 물질

역할	이름	HCID	투입량
반응물	Potassium Carbonate	HCID 11430	—
반응물	Dimethylacetamide	HCID 31374	—
반응물	2-Chloropyrimidine	HCID 74404	—
반응물	N-{6-(2-aminoethoxy)-5-(3-methoxyphenoxy)pyrimidin-4-yl}-4-tert-butylbenzenesulfonamide hydrochloride	HCID 67654095	—
용매	Ammonium Chloride	HCID 25517	—
생성물	4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(2-pyrimidinylamino)ethoxy}-pyrimidin-4-yl]benzenesulfonamide hydrate	HCID 19689482	161.1%

반응 조건

온도	100 °C

반응 단계

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 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US05589478
출처 데이터셋	uspto-grants-1996_12
ORD ID	ord-bdcd16175ec840488b5a139991da87b5
출처 메모	uspto-grants-1996_12