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Potassium Carbonate → HCID 22938523、化合物

HRID 856715
ノート
印刷プレビュー

反応式

HRID 856715 の反応式
[NH:1]1[CH:5]=[C:4]([C:6]([O:8][CH3:9])=[O:7])[N:3]=[N:2]1.C(=O)([O-])[O-].[K+].[K+].I[CH2:17][CH2:18][CH3:19]>CN(C=O)C>[CH2:17]([N:2]1[N:3]=[C:4]([C:6]([O:8][CH3:9])=[O:7])[CH:5]=[N:1]1)[CH2:18][CH3:19].[CH2:17]([N:1]1[CH:5]=[C:4]([C:6]([O:8][CH3:9])=[O:7])[N:3]=[N:2]1)[CH2:18][CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 178498891HCID 178498891、化合物

生成物 2

HCID 22938523HCID 22938523、化合物HCID 22938529Methyl 1-propyl-1H-1,2,3-triazole-4-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

methyl 1,2,3-triazole-4-carboxylate (17.6 g) was dissolved in DMF (210 ml), potassium carbonate (11.5 g) and iodopropane (14.9 ml) were added to the mixture, and the mixture was stirred for 16 hours at room temperature. After filtration, the solvent was removed under reduced pressure, and water was added to the obtained residue, and the mixture was extracted with methylene chloride. The organic layer was washed with saturated brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to give methyl 2-propyl-1,2,3-triazole-4-carboxylate (10.3 g), methyl 1-propyl-1,2,3-triazole-5-carbonate (3.2 g) and methyl 1-propyl-1,2,3-triazole-4-carboxylate (2.6 g).

後処理

  1. filtrationAfter filtration
  2. customthe solvent was removed under reduced pressure, and water
  3. additionwas added to the obtained residue
  4. extractionthe mixture was extracted with methylene chloride
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customthe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f706a72bc4dc42e98b2ebc9ee97c53fa
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262185B2

反応ノート

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