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

HRID 1733671
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반응식

HRID 1733671 반응식
[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
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참가 물질

5

반응물 3

HCID 243Benzoic AcidHCID 8471TriethylamineHCID 203000021-(p-Chlorobenzenesulfonyloxy)-1,2,3-benzotriazole

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2083de36b3bc4672b2ac2bba248ffa24
출처 데이터셋
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04242507

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