Chloroacetaldehyde → 2-Bromoimidazo[2,1-b][1,3,4]thiadiazole

Temperature

120 °C

20 g of 5-bromo-[1,3,4]thiadiazol-2-ylamine were dissolved in 60 ml of n-butanol. 15 ml of chloroacetaldehyde (55% in water) were added to the solution. The mixture was heated for 3 h at 120° C. After cooling the reaction mixture was poured into a NaHCO3 solution. The mixture was extracted three times with ethylacetate and the organic phase dried with sodium sulphate and evaporated. The resulting material was purified via silica-gel column chromatography using a petroleum ether-ethylacetate gradient. 2.9 g yellow crystals of the desired product were obtained.

1. temperatureAfter cooling the reaction mixture
2. extractionThe mixture was extracted three times with ethylacetate
3. dry with materialthe organic phase dried with sodium sulphate
4. customevaporated
5. customThe resulting material was purified via silica-gel column chromatography

ORD record

ord-12b18c460abd427b84adaa582ddc2f2e

Source dataset

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08389554B2