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Phenol → HCID 22456677, 화합물

HRID 2186479
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HRID 2186479 반응식
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.Cl[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=1.[OH-].[Na+]>C1(C)C=CC=CC=1>[O:7]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
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참가 물질

5

반응물 3

HCID 996PhenolHCID 14798Sodium HydroxideHCID 23392Picolyl chloride hydrochloride

생성물 1

HCID 22456677HCID 22456677, 화합물수율 102.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a mixture of phenol (5.25 g, 55.8 mmol) and 2-chloromethylpyridine hydrochloride (10 g, 61.0 mmol) in 80 mL of toluene was added sodium hydroxide (5.35 g, 134 mmol. The mixture was refluxed for 16 hours. The mixture was washed twice with 60 mL of water. The organic layer was then extracted three times with 25 mL of 6 N HCl. The aqueous layer was made basic with 250 mL of 10% NaOH and extracted three times with 150 mL of CH2Cl2. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound as a yellow oil (10.6 g, 94%). ES (+) MS m/e=186 (M+H).

후처리

  1. temperatureThe mixture was refluxed for 16 hours
  2. washThe mixture was washed twice with 60 mL of water
  3. extractionThe organic layer was then extracted three times with 25 mL of 6 N HCl
  4. extractionextracted three times with 150 mL of CH2Cl2
  5. dry with materialThe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-45c827302e1c43be92007d0be03b2448
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06403792B1

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