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

HRID 1654234
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HRID 1654234 반응식
[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]
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참가 물질

4

반응물 2

HCID 3301EthylenediamineHCID 193901786,6-Dimethyl-2,4-heptadiynyl bromide

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-96febfc75e9e4bd8a853019fd73cbdc4
출처 데이터셋
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05405873

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