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Potassium Hydroxide → HCID 22267595, 화합물

HRID 2298016
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HRID 2298016 반응식
[C:1]1([N:7]2[N:11]=[C:10]([C:12]([O:14][CH3:15])=[O:13])[C:9]([C:16]([O:18]C)=[O:17])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[K+]>CO>[CH3:15][O:14][C:12]([C:10]1[C:9]([C:16]([OH:18])=[O:17])=[N:8][N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:11]=1)=[O:13]
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참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 14344840dimethyl 2-phenyl-2H-1,2,3-triazole-4,5-dicarboxylate

생성물 1

HCID 22267595HCID 22267595, 화합물수율 85%

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
23 °C

실험 절차

A solution of dimethyl 2-phenyl-2H-1,2,3-triazole-4,5-dicarboxylate (0.522 g, 2.00 mmol) in methanol (40 mL) at 23° C. was treated with a solution of KOH (0.236 g, 4.20 mmol) in methanol (5 mL). The resulting solution was stirred at 23° C. for 17 h and partitioned between NaHCO3 (sat. aq. sol.) and ether. The aqueous layer was washed with ether and acidified carefully to pH 1 with HCl (conc.). The resulting mixture, was extracted with EtOAc. The organic extract was washed with brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by radial chromatography (2 mm plate, CH2Cl2-methanol-acetic acid 90:10:1) to afford 0.42 g (85%) of 5-methoxycarbonyl-2-phenyl-2H-1,2,3-triazole-4carboxylic acid.

후처리

  1. custompartitioned between NaHCO3 (sat. aq. sol.) and ether
  2. washThe aqueous layer was washed with ether
  3. extractionThe resulting mixture, was extracted with EtOAc
  4. extractionThe organic extract
  5. washwas washed with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by radial chromatography (2 mm plate, CH2Cl2-methanol-acetic acid 90:10:1)

출처 및 근거

ORD 기록
ord-fdce6ff289cb4506a59c108329a540c6
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06492401B1

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