Nitromethane → (E)-2-(Benzyloxy)-1-(2-methoxyethoxy)-4-(2-nitrovinyl)benzene

HRID 1427030ノート

反応式

HRID 1427030 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][C:16]=1[O:17][CH2:18][CH2:19][O:20][CH3:21])[CH:12]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])(=O)C.[NH4+].[N+:27]([CH3:30])([O-:29])=[O:28]>C(O)(=O)C>[CH2:1]([O:8][C:9]1[CH:10]=[C:11](/[CH:12]=[CH:30]/[N+:27]([O-:29])=[O:28])[CH:14]=[CH:15][C:16]=1[O:17][CH2:18][CH2:19][O:20][CH3:21])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 6375NitromethaneHCID 517165Ammonium AcetateHCID 867303313-(Benzyloxy)-4-(2-methoxyethoxy)benzaldehyde

生成物 1

HCID 86730332(E)-2-(Benzyloxy)-1-(2-methoxyethoxy)-4-(2-nitrovinyl)benzene

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
130 °C

実験手順

3-(Benzyloxy)-4-(2-methoxyethoxy)benzaldehyde described in Production Example 20-2 (17.6 g, 61.5 mmol) was dissolved in acetic acid (49.3 mL), then ammonium acetate (5.69 g, 73.8 mmol) and nitromethane (8.32 mL, 154 mmol) were added under nitrogen atmosphere at room temperature, and the mixture was heated under reflux at 130° C. for 2 hours. The mixture was cooled to room temperature and then the precipitate was collected by filteration and washed with ethanol to quantitatively obtain the title compound.

後処理

  1. temperaturethe mixture was heated
  2. temperatureThe mixture was cooled to room temperature
  3. customthe precipitate was collected by filteration
  4. washwashed with ethanol

出典と根拠

ORDレコード
ord-b43a95b6bbde413d878e934d654a5d39
出典データセット
uspto-grants-2015_01
特許番号
US08933099B2

反応ノート

読み込み中…