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Hydrochloric Acid → 4-(Fluoromethyl)benzoic acid

HRID 1794249
ノート
印刷プレビュー

反応式

HRID 1794249 の反応式
[F:1][CH2:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9]C)=[O:8])=[CH:5][CH:4]=1.[OH-].[Na+].Cl>CO>[F:1][CH2:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([OH:9])=[O:8])=[CH:5][CH:4]=1
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 21866613Methyl 4-(fluoromethyl)benzoate

生成物 1

HCID 139813684-(Fluoromethyl)benzoic acid収率 93.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 200 ml of methanol, 8.68 g of methyl 4-(fluoromethyl)benzoate was dissolved, and 77 ml of aqueous solution of 1 N sodium hydroxide was added dropwise with stirring and cooling. The mixture was then stirred for 3.5 hours at room temperature. After the mixture was acidified with 1 N hydrochloric acid, the precipitated crystals were collected by filtration, and the filtrate was concentrated. The precipitated crystals were combined with the residue obtained by concentrating the filtrate, and water was added thereto. The mixture was extracted with ethyl acetate and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to provide 7.47 g of the objective compound as colorless crystals. M.p. 192–194° C.

後処理

  1. temperaturecooling
  2. stirringThe mixture was then stirred for 3.5 hours at room temperature
  3. filtrationthe precipitated crystals were collected by filtration
  4. concentrationthe filtrate was concentrated
  5. customobtained
  6. concentrationby concentrating the filtrate, and water
  7. additionwas added
  8. extractionThe mixture was extracted with ethyl acetate
  9. dry with materialdried over anhydrous magnesium sulfate
  10. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-1a0b090fc7af426090a5af10d5d0e770
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07022723B2

反応ノート

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