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

HRID 596939

반응식

HRID 596939 반응식
[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]

참가 물질

3

반응물 2

HCID 674Dimethylamine2회HCID 171112-(Dimethylamino)ethyl acrylate

생성물 1

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

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f26630dcb5694a2194e5886f129711f0
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012445

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