Hydrogen Bromide → 2-Bromo-3-methylcyclohexanone

3-Methylcyclohexanone, 22.4 grams, contained in 250 ml. of chloroform and 50 ml. of ethyl acetate, is heated to boiling. A mixture of 98.3 grams of cupric bromide and 50 ml. of ethyl acetate is added and heated to maintain elimination of hydrogen bromide. When all of the hydrogen bromide is evolved, the mixture is heated to its reflux temperature for 15 minutes, filtered and the filtrate evaporated to a small volume. The residue is placed upon an alumina column and eluted with methylene chloride. Evaporation of the eluate yields 35.5 grams of crude 2-bromo-3-methylcyclohexanone suitable for condensation with the triazoles of Examples 1 or 2.

1. temperatureheated
2. temperaturethe mixture is heated to its
3. temperaturereflux temperature for 15 minutes
4. filtrationfiltered
5. customthe filtrate evaporated to a small volume
6. washeluted with methylene chloride
7. customEvaporation of the

ORDレコード

ord-7c6a97486d9e4f05bccccf6db1bad2fd

出典データセット

uspto-grants-1976_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US03954984