2-Bromoethanol → Benzothiazolium, 3-(2-hydroxyethyl)-6-methoxy-2-methyl-, bromide (1:1)

Temperatur

120 °C

A solution of 6-methoxy-2-methylbenzothiazole (1.82 g) and 2-bromoethanol (8.8 g) was stirred and heated in an oil bath at 120° C. for 74 hours. After cooling the reaction mixture to room temperature, adding ethyl acetate (25 ml) and stirring for 1 hour, the solid was filtered and collected. The solid was then dissolved in methanol (50 ml) and charcoal (0.5 g) was added. The charcoal was removed by passing through a pad of Celite. The solution was then concentrated to a small volume and triturated with ethyl acetate (100 ml). The solid was collected, washed with ethyl acetate (2×30 ml) and dried in an oven under high vacuum at 50° C. overnight to obtain 0.9 g (30%) of 4c.

1. temperatureAfter cooling the reaction mixture to room temperature
2. filtrationthe solid was filtered
3. customcollected
4. dissolutionThe solid was then dissolved in methanol (50 ml)
5. additioncharcoal (0.5 g) was added
6. customThe charcoal was removed
7. concentrationThe solution was then concentrated to a small volume
8. customtriturated with ethyl acetate (100 ml)
9. customThe solid was collected
10. washwashed with ethyl acetate (2×30 ml)
11. customdried in an oven under high vacuum at 50° C. overnight

ORD-Eintrag

ord-4be8fcb7fef542c4bbf7109a6c6bf783

Quelldatensatz

uspto-grants-2002_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06368864B1