N-bromobutanimide → HCID 178519006, compound

Temperature

61 °C

To a solution of 1.33 g of 5-chloromethyl-3-hydroxyisoxazole in 2 ml of dimethylformamide were added 2.0 g of N-bromosuccinimide, and then the mixture was heated at 61° C. for 1.5 hours. The reaction mixture was then poured into 100 ml of ice-water and extracted with diethyl ether, after which the ethereal extract was dried over anhydrous sodium sulphate. The solvent was distilled off, leaving crystals, which were recrystallized from a mixture of diisopropyl ether and hexane, giving 4-bromo-5-chloromethyl-3-hydroxyisoxazole, in the form of white crystals melting at 136.5°-138° C. (with decomposition).

1. extractionextracted with diethyl ether
2. extractionafter which the ethereal extract
3. dry with materialwas dried over anhydrous sodium sulphate
4. distillationThe solvent was distilled off
5. customleaving crystals, which
6. customwere recrystallized from a mixture of diisopropyl ether and hexane

ORD record

ord-bac0d955235c4e8fa7cbed9c4b440298

Source dataset

uspto-grants-1990_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04892882