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

HRID 1886499

反応式

HRID 1886499 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 108521644-(4-Phenoxyphenoxy)benzoic acid収率 92.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒

実験手順

A slurry of 5.00 g (15.6 mmoles) of methyl 4-(4-phenoxyphenoxy)benzoate from Example A, 0.28 g (50.0 mmoles) 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 homogeneous. 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.

後処理

  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

出典と根拠

ORDレコード
ord-1363c0a98aec4abaa776dc70271a76e5
出典データセット
uspto-grants-1992_09
特許番号
US05151489

関連ノート

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