Hydrogen Bromide → 2-Bromo-3-methylcyclohexanone

HRID 1076122

반응식

HRID 1076122 반응식
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4](=[O:8])[CH2:3]1.C(Cl)(Cl)Cl.[BrH:13]>C(OCC)(=O)C>[Br:13][CH:3]1[CH:2]([CH3:1])[CH2:7][CH2:6][CH2:5][C:4]1=[O:8]

참가 물질

5

반응물 3

HCID 260Hydrogen Bromide2회HCID 6212ChloroformHCID 115673-Methylcyclohexanone

생성물 1

HCID 215419562-Bromo-3-methylcyclohexanone

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d95861bcf9bd4edf8a662d1742418443
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03954981

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