Hydrogen Bromide → HCID 15672517, compound

At 5° to 10° C., 225 g (1.46 mol) of cyclopropyl-2-thienylcarbinol was hydrobromic dripped over a period of 1 hour into 972 ml of 48% strengh hydrobromic acid. The mixture was kept for 2 hours at room temperature, after which the organic phase was separated off and the aqueous solution was extracted three times, each time with 300 ml of dichloromethane. The combined organic phases were washed neutral with dilute sodium hydroxide solution and water, dried over magnesium sulfate and evaporated down under reduced pressure. There was obtained 322 g (94%, corrected) of crude bromide (GC: 92%). 1H-NMR (250 MHZ, CDCl3): δ=2.65-2.80 (m, 2H), 3.46 (t, 2H), 5.90-6.10 (m, 1H), 6.61 (d, 1H), 6.80-7.00 (m, 2H), 7.14 (d, 1H).

1. customafter which the organic phase was separated off
2. extractionthe aqueous solution was extracted three times
3. washThe combined organic phases were washed neutral with dilute sodium hydroxide solution and water
4. dry with materialdried over magnesium sulfate
5. customevaporated down under reduced pressure

ORD record

ord-b20bffd45a0147ff8f48cebd78293310

Source dataset

uspto-grants-1993_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05228896