1,2-Dibromoethane → HCID 21833679, 화합물

HRID 2292666노트

반응식

HRID 2292666 반응식
[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=2)[CH:5]=[CH:4][CH:3]=[N:2]1.[Br:14][CH2:15][CH2:16]Br.[OH-].[Na+]>O>[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([O:13][CH2:16][CH2:15][Br:14])=[CH:9][CH:8]=2)[CH:5]=[CH:4][CH:3]=[N:2]1

참가 물질

5

반응물 3

HCID 78391,2-DibromoethaneHCID 14798Sodium HydroxideHCID 1334121-(4-Hydroxybenzyl)pyrazole

생성물 1

HCID 21833679HCID 21833679, 화합물수율 47.3%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a mixture of 4-(1-pyrazolyl)methylphenol (15 g), 32.35 g of 1,2-dibromoethane and water (150 ml) was added dropwise an aqueous solution of sodium hydroxide (4.13 g) dissolved in water (30 ml) while stirring under heating at reflux over 30 minutes. The reaction mixture was then heated at reflux under stirring for further 1 hour, and then cooled to room temperature, which was extracted with diethyl ether (300 ml). The organic layer was washed with 5N aqueous sodium hydroxide solution and then water, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, which afforded 2-[4-(1-pyrazolyl)methylphenoxy]ethyl bromide (11.44 g) as white crystals. Yield, 47%.

후처리

  1. temperatureunder heating
  2. temperatureat reflux over 30 minutes
  3. temperatureThe reaction mixture was then heated
  4. temperatureat reflux
  5. stirringunder stirring for further 1 hour
  6. extractionwhich was extracted with diethyl ether (300 ml)
  7. washThe organic layer was washed with 5N aqueous sodium hydroxide solution
  8. dry with materialwater, dried with anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-06caa3b9fcde44b1a0e5970ccf252d3b
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05684022

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