Hydrochloric Acid → 4-(5-Fluoro-2-(methyloxy)-4-pyridinyl)-3-((methyloxy)carbonyl)benzoic acid

HRID 1662537ノート

反応式

HRID 1662537 の反応式
[F:1][C:2]1[C:3]([C:10]2[CH:15]=[CH:14][C:13]([C:16]([O:18]C)=[O:17])=[CH:12][C:11]=2[C:20]([O:22][CH3:23])=[O:21])=[CH:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[OH-].[K+].Cl>C1COCC1.CO>[F:1][C:2]1[C:3]([C:10]2[CH:15]=[CH:14][C:13]([C:16]([OH:18])=[O:17])=[CH:12][C:11]=2[C:20]([O:22][CH3:23])=[O:21])=[CH:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 57706068Dimethyl 4-(5-fluoro-2-(methyloxy)-4-pyridinyl)-1,3-benzenedicarboxylate

生成物 1

HCID 574675964-(5-Fluoro-2-(methyloxy)-4-pyridinyl)-3-((methyloxy)carbonyl)benzoic 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 83.21A (0.860 g, 2.7 mmol) in THF (7.00 mL) and MeOH (7.00 mL) at 0° C. was added potassium hydroxide (1.5 mL, 3.0 mmol) slowly to maintain the temperature below 6° C. The reaction mixture was allowed to warm to room temperature and stirred for 17 hours. After which, the reaction was 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 83.21B as a colorless solid (0.82 g, 100% yield).

後処理

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

出典と根拠

ORDレコード
ord-0811189dcd3b4d11bbcada8cf4e47215
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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