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Water → 2-Aminoresorcinol ditosylate

HRID 337342
ノート
印刷プレビュー

反応式

HRID 337342 の反応式
[NH2:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9].C(N([CH2:15][CH3:16])CC)C.[C:17]1([CH3:27])[CH:22]=[CH:21][C:20]([S:23](Cl)(=[O:25])=[O:24])=[CH:19][CH:18]=1.[OH2:28]>ClCCl>[CH3:27][C:17]1[CH:22]=[CH:21][C:20]([S:23]([O:9][C:3]2[CH:4]=[CH:5][CH:6]=[C:7]([O:8][S:23]([C:20]3[CH:21]=[CH:22][C:15]([CH3:16])=[CH:18][CH:19]=3)(=[O:24])=[O:28])[C:2]=2[NH2:1])(=[O:25])=[O:24])=[CH:19][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 694512-Aminoresorcinol

生成物 1

HCID 867032532-Aminoresorcinol ditosylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

100 mg of 2-aminobenzene-1,3-diol was dissolved in 2 ml of dichloromethane, and 234 μl of triethyl amine and 320 mg of p-toluene sulfonyl chloride were added and stirred at room temperature for 1.5 hours. To the reaction mixture, 20 ml of water was added, and extracted with 20 ml of ethyl acetate. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and purified by silica gel column chromatography (hexane:ethyl acetate=4:1) to yield 278.1 mg of the title compound.

後処理

  1. extractionextracted with 20 ml of ethyl acetate
  2. dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. custompurified by silica gel column chromatography (hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-2d8aa5891f7b4dbcbda57d5c695a9ac8
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889727B2

反応ノート

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