반응 #1807214

반응 방정식

1,3-dihydro-6-fluoro-2,1-benzisothiazole-2,2-dioxide

ethyl chloroformate

→

1-ethoxycarbonyl-1,3-dihydro-6-fluoro-2,1-benzisothiazole 2,2-dioxide

수율 87.1%

용매

pyridine

반응 조건

후처리

1. 1
   농축concentrated in vacuo
2. 2
   workup.ADDITIONCold hydrochloric acid was added to the precipitate (pH=6)
3. 3
   추출The resulting solution was extracted with ethyl acetate
4. 4
   세척The organic layer was washed with water
5. 5
   건조dried over magnesium sulfate
6. 6
   기타The crude product was purified by silica gel column chromatography (methylene chloride-ethyl acetate 95:5)

실험 절차

To a stirred solution of 1,3-dihydro-6-fluoro-2,1-benzisothiazole-2,2-dioxide (2.57 g) in anhydrous pyridine (8 ml) was added ethyl chloroformate (1.79 g) at 0° C. under N2 atmosphere. The mixture was stirred for 30 minutes and concentrated in vacuo. Cold hydrochloric acid was added to the precipitate (pH=6). The resulting solution was extracted with ethyl acetate. The organic layer was washed with water and dried over magnesium sulfate. The crude product was purified by silica gel column chromatography (methylene chloride-ethyl acetate 95:5) to give 1-ethoxycarbonyl-1,3-dihydro-6-fluoro-2,1-benzisothiazole 2,2-dioxide (3.1 g).

출처