Bromide ion → HCID 15075480, Verbindung

Triphenylphosphane dibromide (5.52 g, 14.41 mmol) was suspended in abs. acetonitrile (15 ml) under argon, the suspension was brought to 19° C. in a water batch and 2-(benzofuran-3-yl)ethanol (2.11 g, 13.1 mmol), dissolved in abs. acetonitrile (7 ml) was added in the course of 15 min. During the addition the temperature of the reaction mixture was kept between 19 and 21° C. The mixture was then left to stand for 12 h without further cooling. The triphenylphosphane which had precipitated out during this period of time was removed from the reaction mixture by filtration. The filtrate obtained was concentrated. For complete removal of the phosphane, the residue obtained was taken up in cyclohexane (20 ml) and the mixture was filtered over a layer of silica gel (15 g) about 3 cm thick. The silica gel was washed with cyclohexane (5×20 ml). The solution obtained in t his way, which contains the desired bromide in a pure form, was concentrated on a rotary evaporator. This was isolated in a yield of 2.47 g (87%) as a yellowish oil.

1. dissolutiondissolved in abs
2. additionDuring the addition the temperature of the reaction mixture
3. customwas kept between 19 and 21° C
4. waitThe mixture was then left
5. customThe triphenylphosphane which had precipitated out during this period of time
6. customwas removed from the reaction mixture by filtration
7. customThe filtrate obtained
8. concentrationwas concentrated
9. customFor complete removal of the phosphane
10. customthe residue obtained
11. filtrationthe mixture was filtered over a layer of silica gel (15 g) about 3 cm thick
12. washThe silica gel was washed with cyclohexane (5×20 ml)
13. customThe solution obtained in t his way, which
14. concentrationwas concentrated on a rotary evaporator
15. customThis was isolated in a yield of 2.47 g (87%) as a yellowish oil

ORD-Eintrag

ord-ded73b5014ac41e0a04aa472e29e845c

Quelldatensatz

uspto-grants-2012_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08138187B2