Hydrochloric Acid → 3-(4-Fluorophenyl)-2,2-dimethylpropanoic acid

HRID 1592331ノート

反応式

HRID 1592331 の反応式
C([O:3][C:4](=[O:16])[C:5]([CH3:15])([CH3:14])[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=1)C.[OH-].[Na+].Cl>O>[F:13][C:10]1[CH:9]=[CH:8][C:7]([CH2:6][C:5]([CH3:15])([CH3:14])[C:4]([OH:16])=[O:3])=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 69423048Ethyl 3-(4-fluorophenyl)-2,2-dimethylpropanoate

生成物 1

HCID 223502093-(4-Fluorophenyl)-2,2-dimethylpropanoic acid収率 87%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3-(4-fluorophenyl)-2,2-dimethylpropionic acid ethyl ester (10.0 g, 44.6 mmol, see Part 1 of Example 25a) and a solution of sodium hydroxide (25 g) in water (110 mL) was heated at reflux for 18 h and cooled to room temperature. The solution was stirred on an ice bath and acidified with concentrated aqueous hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and dried under vacuum. The residue was stirred with dichloromethane and filtered, and the filtrate was concentrated to provide an off-white solid (7.60 g, 87%).

後処理

  1. temperatureat reflux for 18 h
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customdried under vacuum
  5. stirringThe residue was stirred with dichloromethane
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-cf126b75a27f4fce8171e2e2b442e4b3
出典データセット
uspto-grants-2007_11
特許番号
US07291744B2

反応ノート

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