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1-Iodopropane → HCID 66958661、化合物

HRID 1984379
ノート
印刷プレビュー

反応式

HRID 1984379 の反応式
[CH2:1](I)[CH2:2][CH3:3].[O-]CC.[Na+].[CH2:9]([C:11]1[NH:15][N:14]=[C:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:12]=1)[CH3:10]>C(O)C>[CH2:2]([C:1]1[N:15]([CH2:11][CH2:9][CH3:10])[N:14]=[C:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:12]=1)[CH3:3]
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 3

HCID 336431-Iodopropane2 回HCID 2723922Sodium ethoxide2 回HCID 80276141H-Pyrazole-3-carboxylic acid, 5-ethyl-, ethyl ester

生成物 1

HCID 66958661HCID 66958661、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒3 回

実験手順

Propyl iodide (0.43 mL, 4.46 mmol) and a solution of sodium ethoxide in ethanol (21%, 0.95 g, 3.27 mmol) were added to a solution of ethyl 5-ethyl-1H-pyrazole-3-carboxylate (0.5 g, 2.97 mmol) in ethanol (5 mL) at ambient temperature. The reaction was stirred overnight, and additional propyl iodide (0.05 mL) and sodium ethoxide in ethanol (21%, 0.1 g) were added. After 3 hours, the solvent was removed under reduced pressure and the residue was partitioned between an aqueous sodium chloride solution and methyl tert-butyl ether. The aqueous phase was extracted with methyl tert-butyl ether twice. The organic phases were combined, dried over sodium sulfate, filtered, and concentrated under reduced pressure to yield impure ethyl 5-ethyl-1-propyl-1H-pyrazole-3-carboxylate.

後処理

  1. waitAfter 3 hours
  2. customthe solvent was removed under reduced pressure
  3. customthe residue was partitioned between an aqueous sodium chloride solution and methyl tert-butyl ether
  4. extractionThe aqueous phase was extracted with methyl tert-butyl ether twice
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b88dd64dbe52455bb3d3686194366f31
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07544697B2

反応ノート

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