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Water → 5-(Hydroxymethyl)-2-iodophenol

HRID 1888711
ノート
印刷プレビュー

反応式

HRID 1888711 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5](O)=[O:6].B.C1COCC1.O>C1COCC1>[OH:6][CH2:5][C:4]1[CH:8]=[CH:9][C:10]([I:11])=[C:2]([OH:1])[CH:3]=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

5

反応物 3

HCID 962WaterHCID 7368543-Hydroxy-4-iodobenzoic acidHCID 2723981Borane;tetrahydrofuran

生成物 1

HCID 185259415-(Hydroxymethyl)-2-iodophenol収率 88%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

To a solution of 3-hydroxy-4-iodobenzoic acid (20.9 g, 79.3 mmol) in anhydrous THF (160 mL) was added 1 M borane THF solution (240 mL, 240 mmol) by small portions, and the mixture was stirred at 60° C. for 2 hr. Water was added to the reaction mixture, and the mixture was extracted twice with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was washed with diisopropyl ether and hexane to give the title compound (17.4 g, yield 88%) as a white solid.

後処理

  1. extractionthe mixture was extracted twice with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. washthe residue was washed with diisopropyl ether and hexane

出典と根拠

ORDレコード
ord-b8e881aa9c4f4ab0a87d087b2603073a
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501804B2

反応ノート

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