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

HRID 384108
ノート
印刷プレビュー

反応式

HRID 384108 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-b5039cb4823e4dc1bcec6c5b7c00649b
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367708B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート