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Ammonia → 1-phenyl-1H-1,2,3-triazole-5-carboxamide

HRID 1506624
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HRID 1506624 반응식
[C:1]1([N:7]2[C:11]([C:12]([OH:14])=O)=[CH:10][N:9]=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C[N:16]1CCOCC1.ClC(OCC(C)C)=O.N.O1CCOCC1>COCCOC>[C:1]1([N:7]2[C:11]([C:12]([NH2:16])=[O:14])=[CH:10][N:9]=[N:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
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참가 물질

7

반응물 5

HCID 222AmmoniaHCID 79724-MethylmorpholineHCID 312751,4-DioxaneHCID 62365Isobutyl chloroformateHCID 28017501-phenyl-1H-1,2,3-triazole-5-carboxylic acid

생성물 1

HCID 184741521-phenyl-1H-1,2,3-triazole-5-carboxamide

시약·촉매·용매 1

HCID 8071
1,2-Dimethoxyethane
용매

실험 절차

To a solution of 1-phenyl-1H-1,2,3-triazole-5-carboxylic acid (1.0 g, 5.6 mmol) and 4-methylmorpholine (0.57 g, 5.6 mmol) in 1,2-dimethoxyethane (5 mL), isobutyl chloroformate (0.77, 5.6 mmol) was added to the mixture. After 30 minutes, ammonia in dioxane (16.8 mL, 8.4 mmol) was added to the reaction. Then it was stirred overnight. The solvent was removed and dissolved in 50 mL of ethyl acetate. The organic layer was washed with brine twice. The organic layer was dried with Na2SO4, filtered and concentrated and used without further purification. MS (m/z) 189 [M+H]+.

후처리

  1. customThe solvent was removed
  2. dissolutiondissolved in 50 mL of ethyl acetate
  3. washThe organic layer was washed with brine twice
  4. dry with materialThe organic layer was dried with Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customused without further purification

출처 및 근거

ORD 기록
ord-e267bd35a98e4a4aac73c3a79838a321
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09220710B2

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