Hydrochloric Acid → 6-(2,6-Difluoro-4-(methylsulfinyl)phenyl)-5-fluoropicolinic acid

HRID 1499556ノート

反応式

HRID 1499556 の反応式
[F:1][C:2]1[CH:7]=[C:6]([S:8]([CH3:10])=[O:9])[CH:5]=[C:4]([F:11])[C:3]=1[C:12]1[N:17]=[C:16]([C:18]([O:20]C)=[O:19])[CH:15]=[CH:14][C:13]=1[F:22].[OH-].[Na+].Cl>C1COCC1.CO>[F:1][C:2]1[CH:7]=[C:6]([S:8]([CH3:10])=[O:9])[CH:5]=[C:4]([F:11])[C:3]=1[C:12]1[N:17]=[C:16]([C:18]([OH:20])=[O:19])[CH:15]=[CH:14][C:13]=1[F:22]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 70655092Methyl 6-(2,6-difluoro-4-(methylsulfinyl)phenyl)-5-fluoropicolinate

生成物 1

HCID 706546086-(2,6-Difluoro-4-(methylsulfinyl)phenyl)-5-fluoropicolinic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 6-[2,6-difluoro-4-(methylsulfinyl)phenyl]-5-fluoropyridine-2-carboxylate (37.0 mg, 0.112 mmol) was dissolved in THF (0.12 mL) and MeOH (0.12 mL), and 1.0 M aq. NaOH (0.56 mL, 0.56 mmol) was then added. The reaction mixture was stirred at room temperature for 50 min. The mixture was then neutralized with HCl (12 M) to pH=7 and concentrated under reduced pressure to remove all the solvents. The residue was dissolved in THF, dried, filtered and concentrated under reduced pressure to give the sub-title compound as a white powder. LCMS calc. for C13H9F3NO3S (M+H)+: m/z=316.0. Found: 316.2.

後処理

  1. concentrationconcentrated under reduced pressure
  2. customto remove all the solvents
  3. dissolutionThe residue was dissolved in THF
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a3bb71bb20c047a497f33cc37ee29cdd
出典データセット
uspto-grants-2015_12
特許番号
US09200004B2

反応ノート

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