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

HRID 1725177

반응식

HRID 1725177 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8f7aa04846c84afba83fb4468b1efe6e
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07488832B2

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