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

HRID 1848398

反応式

HRID 1848398 の反応式
[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]

参加物

4

反応物 2

HCID 7515N-MethylanilineHCID 62556Pentaerythritol tetraacrylate

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-c2315b66599847e7bae1f0631c346249
出典データセット
uspto-grants-2015_02
特許番号
US08952190B2

関連ノート

読み込み中…