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2-Phenoxybenzyl alcohol → 5-Iodo-2-((2-phenoxybenzyl)oxy)pyridine

HRID 384108
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인쇄 미리보기

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HRID 384108 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([I:8])=[CH:4][N:3]=1.[O:9]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[CH2:22][OH:23])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>CC(N(C)C)=O>[I:8][C:5]1[CH:6]=[CH:7][C:2]([O:23][CH2:22][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[N:3][CH:4]=1
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참가 물질

4

반응물 2

HCID 36601112-Phenoxybenzyl alcoholHCID 43971762-Chloro-5-iodopyridine

생성물 1

HCID 684280695-Iodo-2-((2-phenoxybenzyl)oxy)pyridine

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
110 °C

실험 절차

To a solution of 2-chloro-5-iodopyridine in dimethylacetamide (2 ml), 300 mg of potassium tert-butoxy and 535 mg of (2-phenoxyphenyl)methanol were added, and the reaction solution was stirred at 110° C. for 4 hours. The reaction solution was cooled, then diluted with a saturated saline solution, extracted with diethyl ether, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue obtained was purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-10:90)) to afford the title compound as a white solid.

후처리

  1. temperatureThe reaction solution was cooled
  2. additiondiluted with a saturated saline solution
  3. extractionextracted with diethyl ether
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe residue obtained
  7. customwas purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-10:90))

출처 및 근거

ORD 기록
ord-b5039cb4823e4dc1bcec6c5b7c00649b
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367708B2

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