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Sodium Azide → HCID 86616332、化合物

HRID 2357796
ノート
印刷プレビュー

反応式

HRID 2357796 の反応式
O[CH2:2][C:3]1[N:4]=[CH:5][N:6]([C:8]2[CH:16]=[CH:15][C:14]([N:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]3=[O:23])=[CH:13][C:9]=2[C:10]([OH:12])=[O:11])[CH:7]=1.[CH3:24][Si](C=[N+]=[N-])(C)C.[N-:31]=[N+:32]=[N-:33].[Na+].C([O-])(O)=O.[Na+]>CO.O=S(Cl)Cl.CN(C=O)C.CCOC(C)=O.O.O1CCOCC1>[N:31]([CH2:2][C:3]1[N:4]=[CH:5][N:6]([C:8]2[CH:16]=[CH:15][C:14]([N:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]3=[O:23])=[CH:13][C:9]=2[C:10]([O:12][CH3:24])=[O:11])[CH:7]=1)=[N+:32]=[N-:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 4

HCID 33557Sodium AzideHCID 167693Trimethylsilyldiazomethane2 回HCID 516892Sodium BicarbonateHCID 66974111HCID 66974111、化合物

生成物 1

HCID 86616332HCID 86616332、化合物

試薬・触媒・溶媒 6

HCID 887Methanol溶媒
HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒
HCID 24386Thionyl Chloride溶媒
HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 2-(4-(hydroxymethyl)-1H-imidazol-1-yl)-5-(2-oxopyridin-1(2H)-yl)benzoic acid prepared above (92 mg, 0.30 mmol) in MeOH (4 mL) and dioxane (2 mL) at room temperature, (trimethylsilyl)diazomethane (2 M in ether, 0.30 mL, 0.60 mmol) was added. After the mixture was stirred at room temperature overnight, more (trimethylsilyl)diazomethane (2 M in ether, 0.40 mL, 0.80 mmol) was added. After stirring for another day, the solution was concentrated in vacuo to give a residue. The residue was dissolved in SOCl2 (4 mL). The solution was stirred at room temperature for 20 min before it was concentrated in vacuo to give a residue, which was then dissolved in DMF (3 mL). To the solution, NaN3 (65 mg, 1.0 mmol) was added. After the mixture was stirred at room temperature for 2 h, water and EtOAc were added, then 5% aq. NaHCO3 was added. The organic layer was separated, dried over Na2SO4, concentrated in vacuo to give methyl 2-(4-(azidomethyl)-1H-imidazol-1-yl)-5-(2-oxopyridin-1(2H)-yl)benzoate (25 mg). MS 351.1 (M+H).

後処理

  1. stirringAfter stirring for another day
  2. concentrationthe solution was concentrated in vacuo
  3. customto give a residue
  4. stirringThe solution was stirred at room temperature for 20 min before it
  5. concentrationwas concentrated in vacuo
  6. customto give a residue, which
  7. stirringAfter the mixture was stirred at room temperature for 2 h
  8. customThe organic layer was separated
  9. dry with materialdried over Na2SO4
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-cbe5decc2e454e6ca380781870052ba9
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07763608B2

反応ノート

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