1-Bromo-2-Chloroethane → HCID 22453776, compound

Temperature

20 °C

1.2 cm3 of 1-bromo-2-chloroethane were run, at a temperature in the region of 20° C., into a stirred solution of 1.47 g of 2-mercaptothiazole and 1.95 g of potassium carbonate in 12.5 cm3 of dimethylformamide. The mixture was subsequently stirred for 2 hours at a temperature in the region of 20° C. The insoluble material was filtered off and washed with 2 times 5 cm3 of dimethylformamide. The filtrate was run onto a mixture of 50 g of crushed ice and 50 cm3 of distilled water, 50 cm3 of ethyl ether were then added and the mixture was stirred and then separated by settling. The aqueous phase was separated by settling and then extracted with 2 times 25 cm3 of ethyl ether. The combined ethereal phases were washed with 2 times 25 cm3 of water and then dried over magnesium sulfate. After filtering through paper, the organic solution was evaporated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 2.11 g of 2-(2-chloroethylthio)thiazole were obtained in the form of a mobile oil with a yellow color.

1. filtrationThe insoluble material was filtered off
2. washwashed with 2 times 5 cm3 of dimethylformamide
3. additionThe filtrate was run onto a mixture of 50 g of crushed ice and 50 cm3 of distilled water, 50 cm3 of ethyl ether
4. additionwere then added
5. stirringthe mixture was stirred
6. customseparated
7. customThe aqueous phase was separated
8. extractionextracted with 2 times 25 cm3 of ethyl ether
9. washThe combined ethereal phases were washed with 2 times 25 cm3 of water
10. dry with materialdried over magnesium sulfate
11. filtrationAfter filtering through paper
12. customthe organic solution was evaporated under reduced pressure (5 kPa) at a temperature in the region of 40° C

ORD record

ord-747ed9bea9c249e7bdc582ea6c3814ad

Source dataset

uspto-grants-2002_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06403610B1