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1,2-Dibromoethane → HCID 22471323, 화합물

HRID 1071250
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HRID 1071250 반응식
[F:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[F:8].C(=O)([O-])[O-].[K+].[K+].[Br:16][CH2:17][CH2:18]Br>C(#N)C>[Br:16][CH2:17][CH2:18][O:9][C:4]1[CH:5]=[CH:6][C:7]([F:8])=[C:2]([F:1])[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 78391,2-DibromoethaneHCID 11430Potassium CarbonateHCID 759273,4-Difluorophenol

생성물 1

HCID 22471323HCID 22471323, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
70 °C

실험 절차

A mixture of 15 g of 3,4-difluorophenol, 23.5 g of potassium carbonate and 60 cm3 of 1,2-dibromoethane in 250 cm3 of acetonitrile was stirred at a temperature in the region of 70° C. for 18 hours. After cooling to about 20° C., the reaction mixture was filtered through Celite and then concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. The residue obtained was purified by chromatography under atmospheric pressure, on a column of silica gel (particle size 70-200μ; diameter 8 cm; mass 400 g), eluting with 40-60° C. petroleum ether. The fractions containing the product were combined and then concentrated to dryness under reduced pressure (2 kPa) in the region of 40° C. 15.7 g of 4-(2-bromoethoxy)-1,2-difluorobenzene were obtained in the form of an oil.

후처리

  1. temperatureAfter cooling to about 20° C.
  2. filtrationthe reaction mixture was filtered through Celite
  3. concentrationconcentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C
  4. customThe residue obtained
  5. customwas purified by chromatography under atmospheric pressure, on a column of silica gel (particle size 70-200μ; diameter 8 cm; mass 400 g)
  6. washeluting with 40-60° C. petroleum ether
  7. additionThe fractions containing the product
  8. concentrationconcentrated to dryness under reduced pressure (2 kPa) in the region of 40° C

출처 및 근거

ORD 기록
ord-883d9760394e49388917cc6f444b7381
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06903217B2

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