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Azobisisobutyronitrile → 11-(Acryloylamino)undecanoic acid

HRID 2088240
ノート
印刷プレビュー

反応式

HRID 2088240 の反応式
[C:1]([O-:6])(=[O:5])[C:2](C)=[CH2:3].C[CH:8]([NH:20][CH3:21])[CH2:9][C:10]1[CH:15]=[CH:14][C:13]2OCCO[C:12]=2[CH:11]=1.C(O)CCC[OH:26].CC(N=N[C:35]([C:38]#N)(C)C)(C#N)C>O.C(O)CC>[C:21]([NH:20][CH2:8][CH2:9][CH2:10][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:3][CH2:2][C:1]([OH:6])=[O:5])(=[O:26])[CH:35]=[CH2:38]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6547AzobisisobutyronitrileHCID 80641,4-ButanediolHCID 87595MethacrylateHCID 24257269Ethylenedioxymethylamphetamine

生成物 1

HCID 23517111-(Acryloylamino)undecanoic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 1031
1-Propanol
溶媒

実験手順

For the preparation of stationary phases, the inner walls of capillaries were vinylized with 3-(trimethoxylsilyppropyl methacrylate. Subsequently, AAUA, EDMA, 1-propanol, 1,4-butanediol, water, and AIBN were mixed ultrasonically into a homogenous solution and purged with nitrogen for 10 min. A 45 cm long silanized capillary was tilled with the polymerization mixture up to a length of 35 cm, sealed with rubber septum, and then placed in a gas chromatography (GC) oven to polymerize for 20 hours at 60° C. The reaction scheme for the polymerization is shown in Scheme 1. Each column of the experimental design was made in duplicate. After the polymerization of the mixture, the monolithic column was washed with methanol for 12 hours using a HPLC pump to remove unreacted monomers and porogens. An on-column detection window was made next to the polymer bed using a thermal wire stripper. Finally, the column was cut to 45 cm with an effective length of 30 cm.

後処理

  1. customFor the preparation of stationary phases
  2. custompurged with nitrogen for 10 min
  3. customsealed with rubber septum
  4. customto polymerize for 20 hours at 60° C
  5. customThe reaction scheme for the polymerization
  6. customAfter the polymerization of the mixture
  7. washthe monolithic column was washed with methanol for 12 hours
  8. customto remove unreacted monomers and porogens

出典と根拠

ORDレコード
ord-30bcf309d103495b8e0eac70c448f4d9
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08435410B2

反応ノート

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