Bromine → HCID 59456287, compound

Temperature

-70 °C

24.3 g (about 0.97 mol) of crude 2-propylselenophene are initially introduced in 100 ml of diethyl ether, and 64.5 ml (0.10 mol, 15% soln. in hexane) of n-BuLi are rapidly metered. The mixture is heated under reflux for 1 h and subsequently cooled to −70° C. 16.5 g (0.10 mol) of bromine are added, and the batch is stirred for 1 h at 0° C. and for 3 h at RT. The mixture is added to semi-conc. sodium hydrogensulfite soln., and the organic phase is separated off. The aqueous phase is extracted with MTBE, and the combined organic phases are washed with sat. sodium chloride soln. The solution is dried using sodium sulfate and concentrated to dryness. The residue is purified by vacuum distillation.

1. temperatureThe mixture is heated
2. temperatureunder reflux for 1 h
3. additionThe mixture is added to semi-conc
4. custom, and the organic phase is separated off
5. extractionThe aqueous phase is extracted with MTBE
6. washthe combined organic phases are washed with sat. sodium chloride soln
7. customThe solution is dried
8. concentrationconcentrated to dryness
9. distillationThe residue is purified by vacuum distillation

ORD record

ord-ce83e9f43406436384e27dff353d4513

Source dataset

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08304036B2