Acetone → Diethyl isophthalate

HRID 1783276ノート

反応式

HRID 1783276 の反応式
BrCCCCCCOC1C=CC(C2C=CC(C#N)=CC=2)=CC=1.O[C:24]1[CH:25]=[C:26]([C:35]([O:37][CH2:38][CH3:39])=[O:36])[CH:27]=[C:28]([CH:34]=1)[C:29]([O:31][CH2:32][CH3:33])=[O:30].CC(C)=O>O>[C:29]([O:31][CH2:32][CH3:33])(=[O:30])[C:28]1[CH:34]=[CH:24][CH:25]=[C:26]([C:35]([O:37][CH2:38][CH3:39])=[O:36])[CH:27]=1

参加物

5

反応物 3

HCID 180AcetoneHCID 6064565-Hydroxy-isophthalic acid diethyl esterHCID 23432392HCID 23432392、化合物

生成物 1

HCID 12491Diethyl isophthalate収率 90%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

0.08 mol (28.8 g) of 4-(6-bromohexyloxy)-4′-cyanobiphenyl, 0.08 mol (16.6 g) of diethyl 5-hydroxyisophthalate, 0.12 mol (19.2 g) of potassium carbonate anhydride and 400 ml of acetone were placed in a 1 l three-neck flask and the mixture was reacted under reflux for 24 hours by using a water bath. After the reaction solution was allowed to cool, it was poured into about 4 l of purified water to take out a precipitate, which was to be a crude subject product, by filtration and the precipitate was dried under reduced pressure (yield: 90% (37 g)). The resulting precipitate was recrystallized from acetone to obtain diethyl isophthalate carrying cyanobiphenyl through a hexyl group as a target product (yield: 73% (30 g)). The resulting compound was subjected to nuclear magnetic resonance (NMR) measurement. The results of measurement are shown below. Also, the compound was subjected to mass spectrometry, with the result that a peak corresponding to a molecular weight of 515.6 was confirmed.

後処理

  1. customthe mixture was reacted
  2. temperatureunder reflux for 24 hours
  3. temperatureto cool
  4. filtrationby filtration
  5. customthe precipitate was dried under reduced pressure (yield: 90% (37 g))
  6. customThe resulting precipitate was recrystallized from acetone

出典と根拠

ORDレコード
ord-4b66bd81feb74d5f85c175b33f2e7d3a
出典データセット
uspto-grants-2009_03
特許番号
US07501210B2

反応ノート

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