Potassium Hydroxide → 2'-Fluoro-2-((methyloxy)carbonyl)-1,1'-biphenyl-4-carboxylic acid

HRID 1662415ノート

反応式

HRID 1662415 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9]([C:18]([O:20][CH3:21])=[O:19])=[CH:10][C:11]([C:14]([O:16]C)=[O:15])=[CH:12][CH:13]=1.[OH-].[K+]>C1COCC1.CO>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([C:14]([OH:16])=[O:15])=[CH:10][C:9]=1[C:18]([O:20][CH3:21])=[O:19]

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 57706591Dimethyl 2'-fluoro-1,1'-biphenyl-2,4-dicarboxylate

生成物 1

HCID 577067632'-Fluoro-2-((methyloxy)carbonyl)-1,1'-biphenyl-4-carboxylic acid収率 95%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 66.32A (1.00 g, 3.5 mmol) in THF (70.0 mL) and MeOH (70.0 mL) at 0° C. was slowly added potassium hydroxide (1.9 mL, 3.8 mmol) to maintain the temperature below 6° C. The reaction mixture was allowed to warm to room temperature and stirred for 48 hours. The reaction mixture was then concentrated in vacuo, acidified with 1N HCl, and extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and to give a white solid 66.32B (0.90 g, 95% yield).

後処理

  1. customat 0° C.
  2. temperatureto maintain the temperature below 6° C
  3. concentrationThe reaction mixture was then concentrated in vacuo
  4. extractionextracted three times with EtOAc
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. filtrationfiltering
  7. customthe organic solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-96503ff0837841a9bc59ec8edb4b8a70
出典データセット
uspto-grants-2011_10
特許番号
US08030354B2

反応ノート

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