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1,2-Dibromoethane → HCID 12725189、化合物

HRID 477493
ノート
印刷プレビュー

反応式

HRID 477493 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([Br:9])[C:3]=1[OH:10].[Br:11][CH2:12][CH2:13]Br.[OH-].[K+]>C(O)C>[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([Br:9])[C:3]=1[O:10][CH2:13][CH2:12][Br: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 78391,2-DibromoethaneHCID 14797Potassium HydroxideHCID 17078p-Cresol, 2,6-dibromo-

生成物 1

HCID 12725189HCID 12725189、化合物収率 65.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2,6-dibromo-4-methylphenol (18) (26.59 g, 0.1 mol), 1,2-dibromoethane (11.2 ml, 0.13 mol) and potassium hydroxide (8.42 g, 0.15 mol) in 200 ml of absolute ethanol was heated under reflux for 24 hours. The inorganic salt was collected on a filter and the filtrate taken to dryness. The resulting mixture was treated with ethyl ether, chilled, and the solid, which proved to be recovered phenol, collected on a filter. The filtrate was evaporated to afford the ether 19 (24.5 g, 65.7%) as a liquid. This was purified by distillation (0.5 torr, 120°-124° C.) to yield 19.79 g (53.0%) of product. NMR (CDCl3) δ 7.25 (s, 2H, aromatic protons), 3.55-4.38 (m, 4H, 2CH2), and 2.27 (s, 3H, CH3).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 24 hours
  3. customThe inorganic salt was collected on
  4. filtrationa filter
  5. additionThe resulting mixture was treated with ethyl ether
  6. temperaturechilled
  7. customto be recovered phenol
  8. customcollected on a filter
  9. customThe filtrate was evaporated

出典と根拠

ORDレコード
ord-d7b47b653e2046e09dcb848af2ba5bbc
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04888353

反応ノート

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