Hydrochloric Acid → HCID 54230354、化合物

HRID 437812ノート

反応式

HRID 437812 の反応式
[OH:1]O.[F:3][C:4]1[CH:25]=[CH:24][C:7]([O:8][C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=2[CH2:18][C:19](=[O:23])C(O)=O)=[CH:6][CH:5]=1.Cl>[OH-].[Na+]>[F:3][C:4]1[CH:5]=[CH:6][C:7]([O:8][C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=2[CH2:18][C:19]([OH:23])=[O:1])=[CH:24][CH:25]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 214270062-(4-Fluorophenoxy)-5-nitro-α-oxobenzenepropanoic acid

生成物 1

HCID 54230354HCID 54230354、化合物

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
25 °C

実験手順

560 Ml. of a 10% aqueous solution of hydrogen peroxide are added dropwise at 0° over a period of 75 minutes to a solution of 142 g. of 2 -(4-fluoro-phenoxy)-5-nitro-phenylpyruvic acid in 2.23 liters of 10% sodium hydroxide solution cooled to 0° C. The mixture is subsequently stirred for 3 hours at 25° C. and then acidified with 500 ml. of concentrated hydrochloric acid with cooling. This mixture is extracted twice with methylene chloride. The methylene chloride solutions are washed with water, dried over sodium sulfate and concentrated in vacuo. The residue is crystallized from benzene/hexane, and there is obtained 2-(4-fluoro-phenoxy)-5-nitro-phenylacetic acid having a melting point of 129°-130° C.

後処理

  1. extractionThis mixture is extracted twice with methylene chloride
  2. washThe methylene chloride solutions are washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is crystallized from benzene/hexane

出典と根拠

ORDレコード
ord-d1ffb0d0c27c4c8d98b312e150992ccc
出典データセット
uspto-grants-1977_06
特許番号
US04032525

反応ノート

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