Dimethylformamide → 1,3-Dibromo-2-(2-chloroethoxy)-5-fluorobenzene

HRID 928643ノート

反応式

HRID 928643 の反応式
CN(C=O)C.Br[CH2:7][CH2:8][Cl:9].C(=O)([O-])[O-].[K+].[K+].[Br:16][C:17]1[CH:22]=[C:21]([F:23])[CH:20]=[C:19]([Br:24])[C:18]=1[OH:25]>C(OCC)(=O)C>[Br:16][C:17]1[CH:22]=[C:21]([F:23])[CH:20]=[C:19]([Br:24])[C:18]=1[O:25][CH2:7][CH2:8][Cl:9]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 78491-Bromo-2-ChloroethaneHCID 11430Potassium CarbonateHCID 676542,6-Dibromo-4-fluorophenol

生成物 1

HCID 108304061,3-Dibromo-2-(2-chloroethoxy)-5-fluorobenzene収率 56%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

DMF (50 mL), 1-bromo-2-chloroethane (1.0 mL, 12 mmol), and potassium carbonate (1.7 g, 12 mmol) were added to 2,6-dibromo-4-fluorophenol (3.0 g, 11 mmol), and stirred at 50° C. overnight. Ethyl acetate was used as an extraction solvent, and after washing with water and saturated brine, and the resultant was dried over magnesium sulfate. The solvent was distilled away under reduced pressure. The resulting residue was purified by silica gel column chromatography to thus obtain the title compound.

後処理

  1. washafter washing with water and saturated brine
  2. dry with materialthe resultant was dried over magnesium sulfate
  3. distillationThe solvent was distilled away under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-e6e5b6ac665147d0a951ee8243fb0b58
出典データセット
uspto-grants-2016_03
特許番号
US09290487B2

反応ノート

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