Bromine → 4-Bromo-2,3-difluoroaniline

温度

0 °C

2,3-difluoro-phenylamine (13.45 g, 104.2 mmol) was diluted with acetic acid (180 ml), bromine (2.6 ml) diluted with acetic acid (5 ml) was slowly added thereto at 0° C., and the solution was stirred for 5 hours. The resulting solution was distilled under a reduced pressure to remove the solvent, basified by adding 50% sodium hydroxide solution (250 ml), and extracted with dichloromethane (200 ml) twice. The separated organic layer was dried over magnesium sulfate, filtered and distilled under a reduced pressure to obtain the title compound 6.46 g (yield: 30%).

1. additionwas slowly added
2. distillationThe resulting solution was distilled under a reduced pressure
3. customto remove the solvent
4. additionby adding 50% sodium hydroxide solution (250 ml)
5. extractionextracted with dichloromethane (200 ml) twice
6. dry with materialThe separated organic layer was dried over magnesium sulfate
7. filtrationfiltered
8. distillationdistilled under a reduced pressure

ORDレコード

ord-d65d2911c30a4fca89e708266d8929ec

出典データセット

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08846699B2