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

HRID 275236
ノート
印刷プレビュー

反応式

HRID 275236 の反応式
[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]
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 7993N,N-Dimethyl-1,3-propanediamineHCID 66986Myristoyl chloride

生成物 1

HCID 170759Myristamidopropyl Dimethylamine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f3e0221111b143b4bf96a6ebd653cbc0
出典データセット
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05393491

反応ノート

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