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Carbon Dioxide → (5-Chloro-2-ethyl-1h-imidazol-4-yl)methanol

HRID 439605
ノート
印刷プレビュー

反応式

HRID 439605 の反応式
[Cl:1][O-].[Na+].[CH2:4]([C:6]1[NH:7][C:8]([CH2:13][OH:14])=[C:9](CO)[N:10]=1)[CH3:5].C(=O)=O>O>[CH2:4]([C:6]1[NH:7][C:8]([CH2:13][OH:14])=[C:9]([Cl:1])[N:10]=1)[CH3:5]
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 280Carbon DioxideHCID 13608920Ethyl-4,5-bis(hydroxymethyl) imidazoleHCID 23665760Sodium Hypochlorite

生成物 1

HCID 10241096(5-Chloro-2-ethyl-1h-imidazol-4-yl)methanol収率 43%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

11.5 Grams (15 mmol) of an aqueous solution containing 9.7% of sodium hypochlorite was dropwisely added to a solution consisting of 2.53 g (16.2 mmol) of the 2-ethyl-4,5-bis(hydroxymethyl) imidazole and 50 ml of water. After the dropwise addition has been finished, the mixture was stirred at room temperature for one hour, followed by neutralization by the addition of dry ice and further followed by evaporation to dryness under reduced pressure. The resulting solid was extracted with ethanol, the extract was evaporated under reduced pressure, and the resulting solid product was extracted with acetone. 1.48 Grams of the starting 2-ethyl-4,5-bis(hydroxymethyl) imidazole was recovered as an extraction residue, the extract was concentrated under reduced pressure, and was subjected to the column chromatography (silica gel-acetone) to obtain a 2-ethyl-4-chloro-5-(hydroxymethyl) imidazole in an amount of 0.46 g (yield 43.0% with respect to the starting material consumed). The TLC and spectra were measured to be the same as those of Example 3.

後処理

  1. additionwas dropwisely added to a solution
  2. additionAfter the dropwise addition
  3. customfurther followed by evaporation to dryness under reduced pressure
  4. extractionThe resulting solid was extracted with ethanol
  5. customthe extract was evaporated under reduced pressure
  6. extractionthe resulting solid product was extracted with acetone
  7. custom1.48 Grams of the starting 2-ethyl-4,5-bis(hydroxymethyl) imidazole was recovered as an extraction residue
  8. concentrationthe extract was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-8294d8a4f47b4a94969cbf3faa657092
出典データセット
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05514811

反応ノート

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