Hydrochloric Acid → 2',5'-Difluoro-2-((methyloxy)carbonyl)-1,1'-biphenyl-4-carboxylic acid

HRID 1662546ノート

反応式

HRID 1662546 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C:9]1[C:10]([C:19]([O:21][CH3:22])=[O:20])=[CH:11][C:12]([C:15]([O:17]C)=[O:16])=[CH:13][CH:14]=1.[OH-].[K+].Cl>C1COCC1.CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([C:15]([OH:17])=[O:16])=[CH:11][C:10]=1[C:19]([O:21][CH3:22])=[O:20]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 57707138Dimethyl 2',5'-difluoro-1,1'-biphenyl-2,4-dicarboxylate

生成物 1

HCID 577063522',5'-Difluoro-2-((methyloxy)carbonyl)-1,1'-biphenyl-4-carboxylic acid収率 100%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 83.27A (0.800 g, 2.6 mmol) in THF (7.00 mL) and MeOH (7.00 mL) at 0° C. was slowly added potassium hydroxide (1.4 mL, 2.9 mmol) to maintain the temperature below 6° C. The reaction mixture was then allowed to warm to room temperature and stirred for 19 hours. The reaction was then 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 to yield 83.27B as a colorless solid (0.76 g, 100% yield).

後処理

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

出典と根拠

ORDレコード
ord-e9a4f0a4b1344172958b7c7db58c5b00
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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