Hydrochloric Acid → 2-methoxy-5-(trifluoromethoxy)benzoic Acid

HRID 339507

反応式

HRID 339507 の反応式
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:8]([O:11][C:12]([F:15])([F:14])[F:13])=[CH:7][C:4]=1[CH:5]=[O:6].[OH-:16].[K+].OO.Cl>CO>[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:8]([O:11][C:12]([F:13])([F:14])[F:15])=[CH:7][C:4]=1[C:5]([OH:16])=[O:6]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14797Potassium HydroxideHCID 27833642-Methoxy-5-(trifluoromethoxy)benzaldehyde

生成物 1

HCID 27752862-methoxy-5-(trifluoromethoxy)benzoic Acid収率 91%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

To a stirred solution of 2-methoxy-5-trifluoromethoxybenzaldehyde (2.0 g, 9.09 mmol) and 50% KOH (4.1 ml) in MeOH (15 ml) at 65° C. was added dropwise hydrogen peroxide (30%, 7.4 ml) over 20 min. The reaction mixture was then stirred at 65° C. for 10 min., cooled to room temperature, acidified with 1 M HCl, and extracted with Et2O (3×40 ml). The combined organic extracts were washed with brine (35 ml), dried (Na2SO4) and the solvent removed under reduced pressure to give a pale yellow viscous oil which solidified at room temperature overnight to give the title compound (1.95 g, 91%) as a pale yellow solid.

後処理

  1. temperaturecooled to room temperature
  2. extractionextracted with Et2O (3×40 ml)
  3. washThe combined organic extracts were washed with brine (35 ml)
  4. dry with materialdried (Na2SO4)
  5. customthe solvent removed under reduced pressure
  6. customto give a pale yellow viscous oil which
  7. waitsolidified at room temperature overnight

出典と根拠

ORDレコード
ord-42d02c996db540dcaa03b8c4c3c23326
出典データセット
uspto-grants-2014_11
特許番号
US08895313B2

関連ノート

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