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N,N-Dimethyl-1,3-propanediamine → Myristamidopropyl Dimethylamine

HRID 1780533
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인쇄 미리보기

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HRID 1780533 반응식
[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][CH2:5][NH2:6].[C:8](Cl)(=[O:22])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]>C(Cl)(Cl)Cl>[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][CH2:5][NH:6][C:8](=[O:22])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7993N,N-Dimethyl-1,3-propanediamineHCID 66986Myristoyl chloride

생성물 1

HCID 170759Myristamidopropyl Dimethylamine

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

2.0 g. (0.0196 moles) of 3-dimethylaminopropylamine in 40 ml chloroform was added dropwise to an ice cold chloroform solution (50 ml) of myristoyl chloride (4.17 g., 0.0169 moles). After addition, the ice bath was removed and the solution was stirred for 2 hours. A 25 ml aqueous sodium bicarbonate solution was added and stirred for 30 minutes. The organic layer was then washed with 30 ml aqueous sodium bicarbonate/sodium chloride solution and dried with magnesium sulfate. The solution was concentrated in vacuo and the amide was recrystallized in ethyl acetate to yield 3.29 g. (0.0105 moles, 62.3%) of the subject compound.

후처리

  1. additionAfter addition
  2. customthe ice bath was removed
  3. additionA 25 ml aqueous sodium bicarbonate solution was added
  4. stirringstirred for 30 minutes
  5. washThe organic layer was then washed with 30 ml aqueous sodium bicarbonate/sodium chloride solution
  6. dry with materialdried with magnesium sulfate
  7. concentrationThe solution was concentrated in vacuo
  8. customthe amide was recrystallized in ethyl acetate
  9. customto yield 3.29 g

출처 및 근거

ORD 기록
ord-8f8dc116d7024950b7af2558a84adc0f
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05631005

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