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Benzoic Acid → 1-(Benzoyloxy)-1H-1,2,3-benzotriazole

HRID 1733671
ノート
印刷プレビュー

反応式

HRID 1733671 の反応式
[C:1]([OH:9])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.ClC1C=CC(S(O[N:28]2[C:32]3[CH:33]=[CH:34][CH:35]=[CH:36][C:31]=3[N:30]=[N:29]2)(=O)=O)=CC=1>C(Cl)(Cl)Cl>[C:1]([O:9][N:28]1[C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][C:31]=2[N:30]=[N:29]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物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 243Benzoic AcidHCID 8471TriethylamineHCID 203000021-(p-Chlorobenzenesulfonyloxy)-1,2,3-benzotriazole

生成物 1

HCID 5552441-(Benzoyloxy)-1H-1,2,3-benzotriazole収率 81.6%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

Benzoic acid (2.44 g) is dissolved in chloroform (30 ml), and thereto are added triethylamine (2.80 ml) under ice-cooling and further 1-(p-chlorobenzenesulfonyloxy)-1,2,3-benzotriazole (6.2 g) at room temperature, and the mixture is stirred for 2 hours. After the reaction, chloroform is distilled off, and to the resulting residue are added water and ethyl acetate. The ethyl acetate layer is washed with water, an aqueous sodium hydrogen sulfate and water in order and dried over anhydrous magnesium sulfate. After drying, the solvent is distilled off to give yellow crystals of 1-benzoyloxy-1,2,3-benzotriazole (3.9 g). The product is recrystallized from isopropanol to give faint yellow crystals of the product, melting point: 75°-78.5° C.

後処理

  1. temperaturecooling
  2. distillationis distilled off
  3. additionto the resulting residue are added water and ethyl acetate
  4. washThe ethyl acetate layer is washed with water
  5. dry with materialan aqueous sodium hydrogen sulfate and water in order and dried over anhydrous magnesium sulfate
  6. customAfter drying
  7. distillationthe solvent is distilled off

出典と根拠

ORDレコード
ord-2083de36b3bc4672b2ac2bba248ffa24
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04242507

反応ノート

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