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

HRID 1884251

反応式

HRID 1884251 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9a3a35f4a44f458b95c06c502bbd9a57
出典データセット
uspto-grants-2004_07
特許番号
US06762321B2

関連ノート

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