Nitroethane → HCID 73877165、化合物

HRID 1743383ノート

反応式

HRID 1743383 の反応式
[CH3:1][O:2][C:3]1[C:10]([CH3:11])=[C:9]([CH3:12])[C:8]([O:13][CH3:14])=[CH:7][C:4]=1[CH:5]=O.C([O-])(=O)C.[NH4+].[N+:20]([CH2:23][CH3:24])([O-:22])=[O:21]>C(OC(C)C)(C)C>[CH3:14][O:13][C:8]1[CH:7]=[C:4]([CH:5]=[C:23]([N+:20]([O-:22])=[O:21])[CH3:24])[C:3]([O:2][CH3:1])=[C:10]([CH3:11])[C:9]=1[CH3:12]

参加物

5

反応物 3

HCID 6587NitroethaneHCID 517165Ammonium AcetateHCID 12629035HCID 12629035、化合物

生成物 1

HCID 73877165HCID 73877165、化合物収率 67%

試薬・触媒・溶媒 1

HCID 7914Diisopropyl Ether溶媒

実験手順

A mixture of 2,5-dimethoxy-3,4-dimethylbenzaldehyde (38.9 g, 0.20 mol), ammonium acetate (10 g, 0.13 mol) and nitroethane (200 mL) was heated to reflux for 2 hours. The reaction mixture was diluted with diisopropyl ether, washed with water and saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was recrystallized from hexane to obtain 33.6 g of the title compound.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. washwashed with water and saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from hexane

出典と根拠

ORDレコード
ord-3f15c87921b147b5a1ee387f0a6eda2b
出典データセット
uspto-grants-2006_03
特許番号
US07008940B1

反応ノート

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