Ethylene Glycol → HCID 56626634、化合物

HRID 66466ノート

反応式

HRID 66466 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([N+:25]([O-:27])=[O:26])[CH2:13][CH2:14][C:15](=[O:24])[CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:39](O)[CH2:40][OH:41]>C1CCCCC1>[CH2:40]1[O:41][C:15]([CH2:16][CH2:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)([CH2:14][CH2:13][CH:12]([N+:25]([O-:27])=[O:26])[CH2:11][C:5]2[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[O:24][CH2:39]1

参加物

5

反応物 3

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 201642191-(3',4'-Dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone

生成物 1

HCID 56626634HCID 56626634、化合物

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

Into a 1 l r.b. flask equipped with a Dean Stark trap was placed 46.4 g (0.12 m) of 1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone, 1.5 g p-toluenesulfonic acid, 50 mL of ethylene glycol and 300 mL of cyclohexane. The mixture was allowed to reflux overnight, then concentrated in vacuo. Dil NaHCO3 solution was added to the residue and extracted with ethyl acetate. The organic layer was backwashed with water, dried over anh. MgSO4, filtered and concentrated under reduced pressure to give 45.3 g of an oil which solidified on drying at room temperature under vacuum.

後処理

  1. customflask equipped with a Dean Stark trap
  2. temperatureto reflux overnight
  3. concentrationconcentrated in vacuo
  4. additionDil NaHCO3 solution was added to the residue
  5. extractionextracted with ethyl acetate
  6. dry with materialdried over anh. MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-cff983f688d644729605de86f7b460a4
出典データセット
uspto-grants-1982_08
特許番号
US04342692

反応ノート

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