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

HRID 928643노트

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HRID 928643 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e6e5b6ac665147d0a951ee8243fb0b58
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290487B2

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