Azobisisobutyronitrile → HCID 17862884, compound

Temperature

80 °C

2.7 g (15.3 mmoles) of N-bromosuccinimide and 0.4 g (2.7 mmoles) of azobisisobutyronitrile were added to a solution of 2.8 g (13.3 mmoles) of 3-bromo-2-methylbenzofuran dissolved in 30 ml of monochlorobenzene. The mixture was stirred at 80° C. for 30 minutes to give rise to a reaction. After confirmation of the disappearance of the raw materials, the reaction mixture was cooled to room temperature. The insolubles were removed by filtration. The filtrate was subjected to vacuum distillation to remove the solvent contained therein. The residue was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein, to obtain 3.0 g (yield: 79.0%) of 3-bromo-2-bromomethylbenzofuran.

1. customto give rise
2. customto a reaction
3. customThe insolubles were removed by filtration
4. distillationThe filtrate was subjected to vacuum distillation
5. customto remove the solvent
6. additionThe residue was poured into water
7. extractionfollowed by extraction with ethyl acetate
8. washThe resulting organic layer was washed with water
9. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
10. distillationThe resulting solution was subjected to vacuum distillation
11. customto remove the solvent

ORD record

ord-624aa9753cbe498d88289e9d8b3758a5

Source dataset

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07833939B2