Iodine → HCID 66733550、化合物

HRID 403011

反応式

HRID 403011 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][C:16]=1[O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:12][OH:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I:25]I>C(Cl)(Cl)Cl.FC(F)(F)C([O-])=O.[Ag+]>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([C:14]([I:25])=[CH:15][C:16]=1[O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:12][OH:13])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 807IodineHCID 743383,4-Bis(benzyloxy)benzyl alcohol

生成物 1

HCID 66733550HCID 66733550、化合物収率 84%

試薬・触媒・溶媒 2

HCID 76299Silver trifluoroacetate触媒HCID 6212Chloroform溶媒2 回

実験手順

The dibenzyloxybenzyl alcohol 28 (21.44 mmol) and silver trifluoroacetate (21.44 mmol) were suspended in 100 mL of dry chloroform and stirred under argon. A solution of iodine (21.44 mmol) in dry chloroform (50 mL) was added to the suspension dropwise at room temperature. The reaction mixture was then stirred for a further period of 2 h and filtered. The filtrate was washed with 20% sodium thiosulfate solution in water. The organic layer was separated and dried over anhydrous Na2SO4. Filtration was followed by evaporation of the chloroform solution resulting in the pure iodo compound, 3,4-Dibenzyloxy-6-iodobenzyl alcohol (29), as a pale yellow solid in 84% yield.

後処理

  1. stirringThe reaction mixture was then stirred for a further period of 2 h
  2. filtrationfiltered
  3. washThe filtrate was washed with 20% sodium thiosulfate solution in water
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationFiltration
  7. customwas followed by evaporation of the chloroform solution

出典と根拠

ORDレコード
ord-ecb27ec953764accb3730e698a8568d6
出典データセット
uspto-grants-2014_06
特許番号
US08742139B2

関連ノート

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