反应 #364579

反应方程式

N-bromosuccinimide

5-amino-6-fluoro-3-methyl-1,2-benzisothiazole

N-bromosuccinimide

→

title compound

收率 101.3%

5-Amino-4-bromo-6-fluoro-3-methyl-1,2-benzisothiazole

收率 101.3%

溶剂

1,2-dichloroethane

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture is stirred 40 minutes at 70° C
2. 2
   温度The mixture is then cooled to room temperature
3. 3
   过滤filtered
4. 4
   浓缩concentrated in vacuo
5. 5
   其他to obtain a residue
6. 6
   其他The residue is chromatographed on silica gel

实验过程

To a solution of 5-amino-6-fluoro-3-methyl-1,2-benzisothiazole (0.600 g, 0.00329 mol) in 1,2-dichloroethane is added N-bromosuccinimide (0.586 g, 0.00329 mol) followed by 1,1′-azobis(cyclohexanecarbonitrile) (0.0200 g). The mixture is stirred two hours at 70° C., additional N-bromosuccinimide (0.240 g, 0.00135 mol) is added, and the mixture is stirred 40 minutes at 70° C. The mixture is then cooled to room temperature, filtered and concentrated in vacuo to obtain a residue. The residue is chromatographed on silica gel to give the title compound (0.870 g, 100%) which is identified by NMR spectral analysis.

来源