Hydrochloric Acid → 4-(4-Phenoxyphenoxy)benzoic acid

HRID 1086585노트

반응식

HRID 1086585 반응식
[O:1]([C:8]1[CH:24]=[CH:23][C:11]([O:12][C:13]2[CH:22]=[CH:21][C:16]([C:17]([O:19]C)=[O:18])=[CH:15][CH:14]=2)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].Cl>CO.O>[O:1]([C:8]1[CH:24]=[CH:23][C:11]([O:12][C:13]2[CH:14]=[CH:15][C:16]([C:17]([OH:19])=[O:18])=[CH:21][CH:22]=2)=[CH:10][CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 19876201Methyl 4-(4-phenoxyphenoxy)benzoate

생성물 1

HCID 108521644-(4-Phenoxyphenoxy)benzoic acid수율 92.1%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매

실험 절차

A slurry of 5.00 g (15.6 mmol) of methyl 4-(4-phenoxyphenoxy)benzoate from Example 30, 0.28 g (50.0 mmol) of potassium hydroxide, 50 ml of methanol and 50 ml of deionized water is refluxed for 48 hours. Methanol is added until the mixture is homogenous. Aqueous hydrochloric acid is added until the solution is strongly acidified, and the slurry is cooled. The resulting precipitate is filtered, washed with 300 ml of deionized water and dried in air. It is recrystallized from a minimum volume of hot 2-1 by volume methanol and water solution to yield 4.40 g (92 percent yield) of 4-(4-phenoxyphenoxy)benzoic acid having a melting point of 185° C. as measured by DSC.

후처리

  1. temperaturethe slurry is cooled
  2. filtrationThe resulting precipitate is filtered
  3. washwashed with 300 ml of deionized water
  4. customdried in air
  5. customIt is recrystallized from a minimum volume of hot 2-1 by volume methanol and water solution

출처 및 근거

ORD 기록
ord-7fb2e42b24cd4bac831a6e7bc78a78c5
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05030706

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