Acetic Acid → 2-Methoxy-4-(2-nitroethenyl)-1-(phenylmethoxy)benzene

HRID 1884251

반응식

HRID 1884251 반응식
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=O)=[CH:11][C:10]=1[O:17][CH3:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N+:19]([CH3:22])([O-:21])=[O:20].C(O)(=O)C.C(N)CCC>C(OCC)(=O)C>[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[CH:22][N+:19]([O-:21])=[O:20])=[CH:11][C:10]=1[O:17][CH3:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 6375NitromethaneHCID 8007ButylamineHCID 755064-(Benzyloxy)-3-methoxybenzaldehyde

생성물 1

HCID 158282-Methoxy-4-(2-nitroethenyl)-1-(phenylmethoxy)benzene수율 62.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

23.1 g (95.7 mmol) of 4-benzyloxy-3-methoxybenzaldehyde, 8.76 g (143 mmol) of nitromethane and 250 ml of acetic acid were mixed and 7.07 g (96.7 mmol) of butylamine was added dropwise thereto. The mixture was refluxed for 2 hours by heating, and then cooled and poured into ice-water. The precipitated crystals were dissolved with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was washed with hexane and dried to give 17.0 g of 1-benzyloxy-2-methoxy-4-(2-nitrovinyl)benzene.

후처리

  1. temperatureThe mixture was refluxed for 2 hours
  2. temperatureby heating
  3. temperaturecooled
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. washThe residue was washed with hexane
  8. customdried

출처 및 근거

ORD 기록
ord-9a3a35f4a44f458b95c06c502bbd9a57
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06762321B2

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