Dimethylamine → 2-(N,N-dimethylamino)ethyl 3-(N',N'-dimethylamino)propionate

HRID 596939

反応式

HRID 596939 の反応式
[CH3:1][NH:2][CH3:3].[C:4]([O:8][CH2:9][CH2:10][N:11]([CH3:13])[CH3:12])(=[O:7])[CH:5]=[CH2:6]>>[CH3:1][N:2]([CH2:6][CH2:5][C:4]([O:8][CH2:9][CH2:10][N:11]([CH3:13])[CH3:12])=[O:7])[CH3:3]

参加物

3

反応物 2

HCID 674Dimethylamine2 回HCID 171112-(Dimethylamino)ethyl acrylate

生成物 1

HCID 214492152-(N,N-dimethylamino)ethyl 3-(N',N'-dimethylamino)propionate

実験手順

Anhydrous dimethylamine (19.8 grams) was added dropwise to 2-(N,N-dimethylamino)ethyl acrylate (31.5 grams) in a magnetically-stirred, ice-cooled reaction vessel at such a rate that the temperature did not exceed 40° C. The addition of dimethylamine was complete in about 10 minutes. After allowing the reaction mixture to stir overnight at room temperature, it was subjected to reduced pressure (about 20 mm. Hg) to remove unreacted dimethylamine. Gas-liquid chromatographic analysis indicated that the residue product was 96.5 per cent pure. The structure of the product, ##STR20## was verified spectroscopically (nuclear magnetic resonance and infrared) and by elemental analysis. Anal. Calc'd. for C9H20N2O2 : C, 57.4; H, 10.6; N, 14.9. Found: C, 57.3; H, 10.5; N, 14.8. This product is designated herein as Amine Catalyst X.

後処理

  1. temperaturecooled
  2. customreaction vessel at such a rate that the temperature
  3. customdid not exceed 40° C
  4. customto remove unreacted dimethylamine

出典と根拠

ORDレコード
ord-f26630dcb5694a2194e5886f129711f0
出典データセット
uspto-grants-1977_03
特許番号
US04012445

関連ノート

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