Hydrochloric Acid → 4-(4-Oxo-4-phenyl-butyryl)-benzoic acid

HRID 1725177

反応式

HRID 1725177 の反応式
C([O:3][C:4](=[O:23])[C:5]1[CH:10]=[CH:9][C:8]([C:11](=[O:22])[CH2:12][CH2:13][C:14](=[O:21])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:7][CH:6]=1)C.[OH-].[K+].Cl>C1COCC1.O>[O:21]=[C:14]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:13][CH2:12][C:11]([C:8]1[CH:9]=[CH:10][C:5]([C:4]([OH:23])=[O:3])=[CH:6][CH:7]=1)=[O:22]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 44520324-(4-Oxo-4-phenyl-butyryl)-benzoic acid ethyl ester

生成物 1

HCID 574236664-(4-Oxo-4-phenyl-butyryl)-benzoic acid収率 45.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a solution of 6.17 g 4-(4-oxo-4-phenyl-butyryl)-benzoic acid ethyl ester from Step 1 in 100 mL THF was added a solution of 3.86 g (69 mmol) potassium hydroxide in 110 mL water. The reaction was heated to reflux for 4.5 hr and allowed to cool. The reaction was transferred to an Ehrlenmeyer flask and cooled to 0° C. in an ice bath. Concentrated hydrochloric acid was added dropwise until a solid precipitated. The solid was collected by filtration and dried to afford 2.59 g (9.1 mmol) 4-(4-oxo-4-phenyl-butyryl)-benzoic acid.

後処理

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 4.5 hr
  3. temperatureto cool
  4. customprecipitated
  5. filtrationThe solid was collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-8f7aa04846c84afba83fb4468b1efe6e
出典データセット
uspto-grants-2009_02
特許番号
US07488832B2

関連ノート

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