تفاعل #1807214

معادلة التفاعل

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

المردود 87.1%

المذيبات

pyridine

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر