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Dibutylamine → N,N-dibutylpentanamide

HRID 1395865
ノート
印刷プレビュー

反応式

HRID 1395865 の反応式
[CH2:1]([NH:5][CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[C:10](Cl)(=[O:15])[CH2:11][CH2:12][CH2:13][CH3:14]>C(OCC)C>[CH2:1]([N:5]([CH2:6][CH2:7][CH2:8][CH3:9])[C:10](=[O:15])[CH2:11][CH2:12][CH2:13][CH3:14])[CH2:2][CH2:3][CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8148Dibutylamine2 回HCID 61186Valeryl chloride

生成物 1

HCID 304103N,N-dibutylpentanamide

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

a round-bottom flask containing a magnetic stirring bar, diethyl ether (400 mL) and N,N-dibutylamine (37 mL, 0.22 mol, 2.2 equiv.) was cooled in ice for 30 minutes. Valeroyl chloride (12.0 mL, 0.099 mol, 1.0 equiv.) was combined with diethyl ether (75 mL) and added dropwise over 30 minutes to the stirring dibutylamine solution on ice. A white precipitate, likely the amine's chloride salt, was observed. The flask was removed from ice and stirred at room temperature for 3 h. Two 500 mL extractions were performed with dilute HCl (10 mL conc. HCl per 500 mL extraction) to remove the excess amine and ammonium chloride byproduct. The diethyl ether layer was retained and dried with MgSO4. Diethyl ether was removed under rotary evaporation and high vacuum, leaving crude N,N-dibutylpentanamide.

後処理

  1. additiona round-bottom flask containing a magnetic stirring bar
  2. customThe flask was removed from ice
  3. extractionTwo 500 mL extractions
  4. customto remove the excess amine and ammonium chloride byproduct
  5. dry with materialdried with MgSO4
  6. customDiethyl ether was removed under rotary evaporation and high vacuum

出典と根拠

ORDレコード
ord-29c0bded4c804bdab46d5171c1f63922
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08900444B2

反応ノート

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