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Hydrochloric Acid → 4-Amino-2-fluoro-3-methylbenzoic acid

HRID 377275
ノート
印刷プレビュー

反応式

HRID 377275 の反応式
[NH2:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8]CC)=[O:7])=[C:4]([F:13])[C:3]=1[CH3:14].[OH-].[Na+].Cl>C(O)C>[NH2:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:13])[C:3]=1[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 19358316Ethyl 4-amino-2-fluoro-3-methylbenzoate

生成物 1

HCID 193583204-Amino-2-fluoro-3-methylbenzoic acid収率 98.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 7 ml of ethanol was suspended 0.70 g of ethyl 4-amino-2-fluoro-3-methylbenzoate, followed by adding thereto 7 ml of lN sodium hydroxide, and the resulting mixture was stirred at 40° C. for 4 hours. To the reaction mixture was added 1.2 ml of 6N hydrochloric acid, followed by extraction with 50 ml of ethyl acetate. The extract solution was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent, to obtain 0.59 g of 4-amino-2-fluoro-3-methylbenzoic acid as colorless crystals.

後処理

  1. additionby adding
  2. extractionfollowed by extraction with 50 ml of ethyl acetate
  3. washThe extract solution was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationdistilled under reduced pressure
  6. customto remove the solvent

出典と根拠

ORDレコード
ord-eb8017b3b8a348f08efb059870b50d3e
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06025370

反応ノート

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