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1,10-Dibromodecane → HCID 19874510、化合物

HRID 465456
ノート
印刷プレビュー

反応式

HRID 465456 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=[O:11])[CH3:10])=[CH:4][CH:3]=1.[Na].[Br:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]Br>CO>[CH2:8]([C:5]1[CH:4]=[CH:3][C:2]([O:1][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][Br:13])=[CH:7][CH:6]=1)[C:9]([CH3:10])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 2214831,10-DibromodecaneHCID 5360545SodiumHCID 70192744-Hydroxyphenylacetone

生成物 1

HCID 19874510HCID 19874510、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of 4-hydroxyphenyl propan-2-one, ethylene ketal (5.26 g) in methanol at room temperature, was treated with sodium (0.66 g) and allowed to stir for 10 minutes. The resulting solution was then added dropwise over 15 minutes to a solution of 1,10-dibromodecane (9.0 g) in methanol under reflux and the reaction mixture heated for 3 h. The mixture was allowed to cool and the solvent was removed in vacuo. The residue was partitioned between diethylether and water, the organic layer separated, dried (magnesium sulphate), and the solvent removed in vacuo to give an oil which was chromatographed on silica. Elution with chloroform gave 10-(4-acetonylphenoxy)decyl bromide, ethylene ketal (3.0 g) as an oil.

後処理

  1. temperatureunder reflux
  2. temperaturethe reaction mixture heated for 3 h
  3. temperatureto cool
  4. customthe solvent was removed in vacuo
  5. customThe residue was partitioned between diethylether and water
  6. customthe organic layer separated
  7. dry with materialdried (magnesium sulphate)
  8. customthe solvent removed in vacuo
  9. customto give an oil which
  10. customwas chromatographed on silica
  11. washElution with chloroform

出典と根拠

ORDレコード
ord-fcfddcfa47c7487293673cf9c020c254
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05153210

反応ノート

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