Propargyl bromide → (Prop-2-yn-1-yl)bis(propan-2-yl)amine

HRID 1068993ノート

反応式

HRID 1068993 の反応式
[CH2:1](Br)[C:2]#[CH:3].[CH:5]([NH:8][CH:9]([CH3:11])[CH3:10])([CH3:7])[CH3:6].C(=O)([O-])[O-].[Cs+].[Cs+]>CC(C)=O>[CH:5]([N:8]([CH:9]([CH3:11])[CH3:10])[CH2:3][C:2]#[CH:1])([CH3:7])[CH3:6]

参加物

5

反応物 3

HCID 7842Propargyl bromideHCID 7912DiisopropylamineHCID 10796Cesium carbonate

生成物 1

HCID 234373(Prop-2-yn-1-yl)bis(propan-2-yl)amine収率 43.7%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Propargyl bromide (23.5 g, 197 mmol) was added dropwise to a mixture of diisopropyl amine (20 g, 197 mmol) and cesium carbonate (64 g, 197 mmol) in 350 mL of acetone. The mixture was stirred overnight under nitrogen at room temperature. The inorganic salts were then filtered off, and the solvent was removed. The residue was dissolved in saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic extracts were then evaporated to give 12 g of diisopropyl-prop-2-ynyl-amine: mass spectrum (m/e): M+H 139.

後処理

  1. filtrationThe inorganic salts were then filtered off
  2. customthe solvent was removed
  3. dissolutionThe residue was dissolved in saturated sodium bicarbonate solution
  4. extractionextracted with ethyl acetate
  5. customThe organic extracts were then evaporated

出典と根拠

ORDレコード
ord-04a454394aee4c8cb564afe2bbf69364
出典データセット
uspto-grants-2001_06
特許番号
US06251912B1

反応ノート

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