2-Bromoethanol → HCID 12016698, compound

Temperature

120 °C

A solution of 2,6-dimethylbenzothiazole (13.0 g) and 2-bromoethanol (100 g) was stirred and heated in an oil bath to 120° C. for 96 hours. After cooling the reaction mixture to room temperature, adding ethyl acetate (150 ml) and stirring for 1 hour, the resultant solid was filtered and collected. The solid was then dissolved in methanol (150 ml) and charcoal (2 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 acetone (200 ml). The solid was collected, washed with acetone (2×30 ml), ethyl acetate (2×30 ml) and dried in an oven under high vacuum at 50 C. overnight to obtain 13.95 g (61%) of 4b.

1. temperatureAfter cooling the reaction mixture to room temperature
2. filtrationthe resultant solid was filtered
3. customcollected
4. dissolutionThe solid was then dissolved in methanol (150 ml)
5. additioncharcoal (2 g) was added
6. customThe charcoal was removed
7. concentrationThe solution was then concentrated to a small volume
8. customtriturated with acetone (200 ml)
9. customThe solid was collected
10. washwashed with acetone (2×30 ml), ethyl acetate (2×30 ml)
11. customdried in an oven under high vacuum at 50 C

ORD record

ord-1dcdf84858ea4621bc2f48fe1de7d521

Source dataset

uspto-grants-2002_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06368864B1