Sodium Chloride → Propanamide, 2,2′-azobis[N-[2-[(2-hydroxyethyl)amino]ethyl]-2-methyl-

HRID 1741227ノート

反応式

HRID 1741227 の反応式
[N:1]([C:10]([CH3:16])([CH3:15])[C:11]([O:13]C)=O)=[N:2][C:3]([CH3:9])([CH3:8])[C:4]([O:6]C)=O.[NH2:17][CH2:18][CH2:19][NH:20][CH2:21][CH2:22][OH:23].[CH3:24][O:25][Na].[Cl-].[Na+]>CO>[N:2]([C:3]([CH3:8])([CH3:9])[C:4]([NH:17][CH2:18][CH2:19][NH:20][CH2:21][CH2:24][OH:25])=[O:6])=[N:1][C:10]([CH3:16])([CH3:15])[C:11]([NH:17][CH2:18][CH2:19][NH:20][CH2:21][CH2:22][OH:23])=[O:13]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 8112N-(2-Hydroxyethyl)ethylenediamineHCID 757631,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate)HCID 178418582HCID 178418582、化合物

生成物 1

HCID 54254381Propanamide, 2,2′-azobis[N-[2-[(2-hydroxyethyl)amino]ethyl]-2-methyl-収率 91.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a constantly stirred mixture comprising 23.0 g of V-601, 22.9 g of 2-(2-aminoethylamino)ethanol and 5 ml of methanol, 4.7 g of 28% CH3ONa was added dropwise. The reaction was carried out with stirring at room temperature for 8 hours. After standing overnight, the reaction mixture was mixed with 50 ml of saturated sodium chloride solution, and extracted with 100 ml of dichloromethane. The organic layer was dried over anhydrous magnesium sulfate and solvent was distilled off, and there was obtained 29.8 g (yield 80%) of 2,2'-azobis [N-(2-hydroxyethylamino)ethyl-2-methylpropionamide ] of yellow viscous liquid.

後処理

  1. additionwas added dropwise
  2. waitAfter standing overnight
  3. extractionextracted with 100 ml of dichloromethane
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate and solvent
  5. distillationwas distilled off

出典と根拠

ORDレコード
ord-03b016fd021244409625e482f549bfb5
出典データセット
uspto-grants-1999_10
特許番号
US05973125

反応ノート

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