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Sodium Methoxide → HCID 68296408、化合物

HRID 631882
ノート
印刷プレビュー

反応式

HRID 631882 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 10942334Sodium MethoxideHCID 68296411HCID 68296411、化合物2 回

生成物 1

HCID 68296408HCID 68296408、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3e2822bc585f4353ad698a33f008b831
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321740B2

反応ノート

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