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2-(3,4-Dimethoxyphenoxy)acetic acid → 1-(1H-Benzo[d][1,2,3]triazol-1-yl)-2-(3,4-dimethoxyphenoxy)ethanone

HRID 710060
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HRID 710060 반응식
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1.[CH3:10][O:11][C:12]1[CH:13]=[C:14]([CH:20]=[CH:21][C:22]=1[O:23][CH3:24])[O:15][CH2:16][C:17](O)=[O:18]>C(Cl)(Cl)Cl.S(Cl)(Cl)=O>[N:1]1([C:17](=[O:18])[CH2:16][O:15][C:14]2[CH:20]=[CH:21][C:22]([O:23][CH3:24])=[C:12]([O:11][CH3:10])[CH:13]=2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1
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참가 물질

5

반응물 2

HCID 218358392-(3,4-Dimethoxyphenoxy)acetic acidHCID 178418385HCID 178418385, 화합물

생성물 1

HCID 867067731-(1H-Benzo[d][1,2,3]triazol-1-yl)-2-(3,4-dimethoxyphenoxy)ethanone수율 109.2%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 24386Thionyl Chloride용매

실험 절차

To a solution of 1H-benzo[d][1,2,3]triazole (11.2 g) in CHCl3 (120 ml), thionyl chloride (1.7 ml) was added and after stirring at room temperature for 30 minutes, 2-(3,4-dimethoxyphenoxy)acetic acid (5.00 g) was added and the mixture was stirred at room temperature for 1.5 hours. The precipitate was filtered off and the filtrate was washed with an aqueous solution of 2 N NaOH; thereafter, the organic layer was dried (MgSO4), filtered and concentrated to give the titled compound (8.06 g, colorless solid.)

후처리

  1. stirringthe mixture was stirred at room temperature for 1.5 hours
  2. filtrationThe precipitate was filtered off
  3. washthe filtrate was washed with an aqueous solution of 2 N NaOH
  4. dry with materialthereafter, the organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3160b0f8570a4c3ca351621bededf526
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181229B2

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