N-Methylaniline → tetra-(hydroxymethyl)methane tetra-(3-[N-methyl-N-phenylamino]propionate)

HRID 1848398

반응식

HRID 1848398 반응식
[C:1]([O:5][CH2:6][C:7]([CH2:20][O:21][C:22](=[O:25])[CH:23]=[CH2:24])([CH2:14][O:15]C(=O)C=C)[CH2:8][O:9]C(=O)C=C)(=[O:4])[CH:2]=[CH2:3].[CH3:26][NH:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>C(O)(=O)C>[CH3:26][N:27]([CH2:24][CH2:23][C:22]([OH:21])=[O:25])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[CH3:26][N:27]([CH2:3][CH2:2][C:1]([OH:5])=[O:4])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[CH3:26][N:27]([CH2:24][CH2:23][C:22]([OH:21])=[O:25])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[CH3:26][N:27]([CH2:24][CH2:23][C:22]([OH:21])=[O:25])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[OH:5][CH2:6][C:7]([CH2:20][OH:21])([CH2:14][OH:15])[CH2:8][OH:9]

참가 물질

4

반응물 2

HCID 7515N-MethylanilineHCID 62556Pentaerythritol tetraacrylate

생성물 1

HCID 67393524tetra-(hydroxymethyl)methane tetra-(3-[N-methyl-N-phenylamino]propionate)

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

Pentaerythritol tetraacrylate (4.4 g, 0.0125 moles) was added to N-methylaniline (5.4 g 0.050 moles), dissolved in glacial acetic acid (10 ml). The mixture was heated with stirring at 100° C. for 2 hours and then the acetic acid removed by vacuum distillation. An infrared spectrum of the residual oil revealed the presence of a little unreacted N-methylaniline but little sign of any unreacted acrylate groups. Absorptions due to the presence of a saturated ester (1730 cm−1) and an aromatic amine (1600 cm−) were found. 1H NMR δ 2.6 (CH2—CO, 8H t), 2.9 (CH3—N 12H s) 3.6 (CH2—N, 8H, t), 4.1 (CH2—O 8H s), 6.7 (aromatic protons 12H) 7.2 (aromatic protons 8H).

후처리

  1. temperatureThe mixture was heated
  2. customthe acetic acid removed by vacuum distillation

출처 및 근거

ORD 기록
ord-c2315b66599847e7bae1f0631c346249
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952190B2

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