반응 #1147209

반응 방정식

N-(2-fluoro-5-(4-methoxypyridin-2-yl)phenyl)-thiourea

sodium hydride

hydrogen chloride

→

2-amino-5-(4-methoxypyridin-2-yl)benzothiazole dihydrochloride

용매

ethyl acetate

dimethyl sulfoxide

1,4-dioxane

ethyl acetate

반응 조건

후처리

1. 1
   세척washed with water three times and brine
2. 2
   건조The separated organic layer was dried over sodium sulfate
3. 3
   기타evaporated under reduced pressure
4. 4
   기타The residue was purified by column chromatography (silica gel 10 g, 5% methanol in dichloromethane)
5. 5
   기타The compound obtained
6. 6
   여과The precipitate was collected by filtration
7. 7
   기타dried under reduced pressure

실험 절차

To a suspension of N-(2-fluoro-5-(4-methoxypyridin-2-yl)phenyl)-thiourea (0.104 g) in dimethyl sulfoxide (5 ml) was added a sodium hydride (60% dispersion in mineral oil ,15.4 mg), and the mixture was stirred at 100° C. for 5 hours. The mixture was diluted with ethyl acetate and washed with water three times and brine. The separated organic layer was dried over sodium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 10 g, 5% methanol in dichloromethane). The compound obtained was dissolved in ethyl acetate, and a solution of hydrogen chloride in 1,4-dioxane (4N, 1 ml) was added. The precipitate was collected by filtration and dried under reduced pressure to give 2-amino-5-(4-methoxypyridin-2-yl)benzothiazole dihydrochloride (46 mg).

출처