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Ethylenediamine → N-(6,6-dimethyl-2,4-heptadiynyl)ethylenediamine

HRID 1654234
ノート
印刷プレビュー

反応式

HRID 1654234 の反応式
[CH2:1]([NH2:4])[CH2:2][NH2:3].[CH3:5][C:6]([CH3:14])([CH3:13])[C:7]#[C:8][C:9]#[C:10][CH2:11]Br>C(O)C>[CH3:5][C:6]([CH3:14])([CH3:13])[C:7]#[C:8][C:9]#[C:10][CH2:11][NH:3][CH2:2][CH2:1][NH2:4]
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 3301EthylenediamineHCID 193901786,6-Dimethyl-2,4-heptadiynyl bromide

生成物 1

HCID 20079885N-(6,6-dimethyl-2,4-heptadiynyl)ethylenediamine収率 63%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 20 ml of ethanol was dissolved 1.5 g of ethylenediamine. Then 1.24 g of 6,6-dimethyl-2,4-heptadiynyl bromide was added to the solution followed by stirring at room temperature overnight. The solvent was distilled off under reduced pressure and the residue was extracted with ethyl ether and saturated sodium bicarbonate aqueous solution. After the organic layer was taken by fractionation, the aqueous layer was further extracted with ethyl ether. The procedure was repeated 5 times and the ethereal layer was dried over anhydrous magnesium sulfate. The drying agent was filtered off and the solvent was then removed under reduced pressure to give 695 mg (yield: 63%) of N-(6,6-dimethyl-2,4-heptadiynyl)ethylenediamine as light yellow oil.

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. extractionthe residue was extracted with ethyl ether and saturated sodium bicarbonate aqueous solution
  3. extractionthe aqueous layer was further extracted with ethyl ether
  4. dry with materialthe ethereal layer was dried over anhydrous magnesium sulfate
  5. filtrationThe drying agent was filtered off
  6. customthe solvent was then removed under reduced pressure

出典と根拠

ORDレコード
ord-96febfc75e9e4bd8a853019fd73cbdc4
出典データセット
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05405873

反応ノート

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