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Sodium Methoxide → HCID 68296408, 화합물

HRID 631882
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HRID 631882 반응식
[CH2:1]([N:8]1[C:12]([C:13]2[C:18]([N+:19]([O-:21])=[O:20])=[CH:17][CH:16]=[CH:15][C:14]=2F)=[N:11][N:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:23][O-:24].[Na+]>C(Cl)Cl.CO>[CH2:1]([N:8]1[C:12]([C:13]2[C:18]([N+:19]([O-:21])=[O:20])=[CH:17][CH:16]=[CH:15][C:14]=2[O:24][CH3:23])=[N:11][N:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 10942334Sodium MethoxideHCID 68296411HCID 68296411, 화합물2회

생성물 1

HCID 68296408HCID 68296408, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

1-Benzyl-5-(2-fluoro-6-nitrophenyl)-1H-tetrazole (Intermediate 18, 0.3 g) was dissolved in DCM (4 mL) and a solution of sodium methoxide in methanol (20%; 2 mL) was added. The mixture was stirred for 4 hours and then the solvent was removed by evaporation under vacuum. The residue was dissolved in ethyl acetate and washed with 1N hydrochloric acid and then brine. The organic solution was dried with sodium sulfate, filtered and the solvent was removed by evaporation under vacuum. The residue was purified by flash chromatography on silica, eluting with a mixture of DCM and methanol. The fractions containing the desired product were combined and evaporated to give the title compound as a pale yellow solid (0.14 g).

후처리

  1. customthe solvent was removed by evaporation under vacuum
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with 1N hydrochloric acid
  4. dry with materialThe organic solution was dried with sodium sulfate
  5. filtrationfiltered
  6. customthe solvent was removed by evaporation under vacuum
  7. customThe residue was purified by flash chromatography on silica
  8. washeluting with a mixture of DCM and methanol
  9. additionThe fractions containing the desired product
  10. customevaporated

출처 및 근거

ORD 기록
ord-3e2822bc585f4353ad698a33f008b831
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321740B2

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