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Methanol → 2-Bromo-1-(1-methylcyclohexyl)ethan-1-one

HRID 1579122
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HRID 1579122 반응식
[Br:1]Br.C(Cl)(Cl)Cl.[CH3:7][C:8]([C:10]1([CH3:16])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)=[O:9].CO>BrBr.O>[CH3:16][C:10]1([C:8]([CH2:7][Br:1])=[O:9])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 887MethanolHCID 6212ChloroformHCID 24408Bromine2회HCID 5441981-(1-methylcyclohexyl)ethanone

생성물 1

HCID 214750112-Bromo-1-(1-methylcyclohexyl)ethan-1-one

시약·촉매·용매 2

HCID 24408Bromine촉매
HCID 962
Water
용매

실험 절차

A solution of 328 g. bromine in 300 ml. chloroform was added gradually to a stirred solution of 300 g. 1-methylcyclohexyl methyl ketone in 100 ml. methanol. After the addition of a few drops of bromine solution at 15°C. the reaction mixture was cooled and maintained between 0°-5°C. The reaction mixture was stirred for 10 minutes, after the addition of bromine had been completed, and then poured on to a mixture of crushed ice and water. The water layer was separated from the organic liquid and extracted with methylene chloride. The extract and the organic portion were combined and washed with water followed by a saturated solution of sodium bicarbonate and then finally with water. After drying over calcium chloride the liquid was evaporated and distilled to give bromomethyl 1-methylcyclohexyl ketone, b.p. 76°-78°C./0.1 mm.Hg.

후처리

  1. temperaturewas cooled
  2. temperaturemaintained between 0°-5°C
  3. customThe water layer was separated from the organic liquid
  4. extractionextracted with methylene chloride
  5. extractionThe extract
  6. washwashed with water
  7. dry with materialAfter drying over calcium chloride the liquid
  8. customwas evaporated
  9. distillationdistilled

출처 및 근거

ORD 기록
ord-32b930b73ba54c8aa33d8552a0db21f5
출처 데이터셋
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03940484

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