Sodium Hydroxide → 2,6-Difluoro-3,5-dimethoxybenzoic acid

HRID 459943ノート

反応式

HRID 459943 の反応式
C[O:2][C:3](=[O:16])[C:4]1[C:9]([F:10])=[C:8]([O:11][CH3:12])[CH:7]=[C:6]([O:13][CH3:14])[C:5]=1[F:15].[OH-].[Na+]>C(O)C>[F:10][C:9]1[C:8]([O:11][CH3:12])=[CH:7][C:6]([O:13][CH3:14])=[C:5]([F:15])[C:4]=1[C:3]([OH:16])=[O:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 59486229Methyl 2,6-difluoro-3,5-dimethoxybenzoate

生成物 1

HCID 184447022,6-Difluoro-3,5-dimethoxybenzoic acid収率 82.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of 115 g (0.49 mol) of 2,6-difluoro-3,5-dimethoxy benzoic acid methyl ester and 42.9 g (1.07 mol) of solid sodium hydroxide in 1.4 L of anhydrous ethanol was refluxed for 24 hours. The ethanol was concentrated in vacuo and the solid residue was dissolved in water and extracted two times with ethyl ether. The aqueous layer was acidified with concentrated hydrochloric acid and a white precipitate was filtered, washed with cold water and dried in vacuo to give 87.9 g (81%) of the title compound. MS (APCI) (m+1)/z 219.1.

後処理

  1. temperaturewas refluxed for 24 hours
  2. concentrationThe ethanol was concentrated in vacuo
  3. dissolutionthe solid residue was dissolved in water
  4. extractionextracted two times with ethyl ether
  5. filtrationa white precipitate was filtered
  6. washwashed with cold water
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-f2d00457297a4452b22bed72baeea1e4
出典データセット
uspto-grants-2007_03
特許番号
US07196090B2

反応ノート

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