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Hydrochloric Acid → 1-(2-Methylphenyl)-1H-1,2,4-triazole-3-carboxylic acid

HRID 1755220
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HRID 1755220 반응식
[C:1]1([CH3:17])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[CH:11]=[N:10][C:9]([C:12]([O:14]CC)=[O:13])=[N:8]1.[Li+].[OH-].CO.Cl>C1COCC1>[C:1]1([CH3:17])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[CH:11]=[N:10][C:9]([C:12]([OH:14])=[O:13])=[N:8]1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 3939Lithium HydroxideHCID 71304241Ethyl 1-(2-methylphenyl)-1H-1,2,4-triazole-3-carboxylate

생성물 1

HCID 713020931-(2-Methylphenyl)-1H-1,2,4-triazole-3-carboxylic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

To a solution of ethyl 1-(o-tolyl)-1,2,4-triazole-3-carboxylate (400 mg, 1.7 mmol) in 3 mL THF was added 4 M LiOH (2 mL, 8 mmol) followed by 3 mL of MeOH. The reaction mixture was stirred at 50° C. for 5 minutes, after which the pH was adjusted to 4 with the addition of conc. HCl. After extraction, drying (MgSO4), filtration and drying under reduced pressure, 43 mg of residue was recovered (12%) and used in the subsequent step without further purification.

후처리

  1. extractionAfter extraction
  2. customdrying
  3. filtration(MgSO4), filtration
  4. dry with materialdrying under reduced pressure, 43 mg of residue
  5. customwas recovered (12%)
  6. customused in the subsequent step without further purification

출처 및 근거

ORD 기록
ord-17a51cb946f349c5b0cc40a8e4901319
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09169261B2

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