Hydrochloric Acid → 5-(3,4-Dimethoxyphenyl)cyclohexane-1,3-dione

HRID 1108754ノート

反応式

HRID 1108754 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]2[CH2:16][C:15](=[O:17])[CH2:14][C:13](=[O:18])[CH:12]2C(OCC)=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].Cl>[OH-].[K+]>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]2[CH2:16][C:15](=[O:17])[CH2:14][C:13](=[O:18])[CH2:12]2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 18784169HCID 18784169、化合物

生成物 1

HCID 8541355-(3,4-Dimethoxyphenyl)cyclohexane-1,3-dione収率 90.7%

試薬・触媒・溶媒 1

HCID 14797Potassium Hydroxide溶媒

反応条件

温度
50 °C

実験手順

10% Aqueous solution of potassium hydroxide (760 ml) was added to ethyl 2-(3,4-dimethoxyphenyl)-4,6-dioxocyclohexane carboxylate (122 g), and the mixture was refluxed for 3.5 hours. After cooling the reaction solution on ice, it was adjusted to pH1 with concentrated hydrochloric acid, and stirred at 50° C. for an hour. After allowing the reaction solution to cool, the deposited crystals were filtered by suction and washed with purified water and isopropyl ether to give 85.8 g of 5-(3,4-dimethoxyphenyl)cyclohexane-1,3-dione (90.5%).

後処理

  1. temperaturethe mixture was refluxed for 3.5 hours
  2. temperatureAfter cooling the reaction solution on ice, it
  3. temperatureto cool
  4. filtrationthe deposited crystals were filtered by suction
  5. washwashed with purified water and isopropyl ether

出典と根拠

ORDレコード
ord-6b7deb2b253a4881818a6a1f4c9b9727
出典データセット
uspto-grants-2000_05
特許番号
US06069176

反応ノート

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