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

HRID 1973265
ノート
印刷プレビュー

反応式

HRID 1973265 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 887MethanolHCID 6212ChloroformHCID 24408Bromine2 回HCID 5441981-(1-methylcyclohexyl)ethanone

生成物 1

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

試薬・触媒・溶媒 2

HCID 24408Bromine触媒
HCID 962
Water
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-88ffa17e74564b98bbcc7c29b17f931d
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03996366

反応ノート

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