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

HRID 1427030노트

반응식

HRID 1427030 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
130 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-b43a95b6bbde413d878e934d654a5d39
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08933099B2

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