Formic Acid → N-(2,6-difluoropyridin-3-yl)formamide

HRID 546780ノート

反応式

HRID 546780 の反応式
C(O[C:5](=[O:7])C)(=O)C.C(O)=O.[F:11][C:12]1[C:17]([NH2:18])=[CH:16][CH:15]=[C:14]([F:19])[N:13]=1.C(=O)(O)[O-].[Na+]>COC(C)(C)C.C(OCC)(=O)C>[F:11][C:12]1[C:17]([NH:18][CH:5]=[O:7])=[CH:16][CH:15]=[C:14]([F:19])[N:13]=1

参加物

7

反応物 4

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 450800062,6-Difluoropyridin-3-amine

生成物 1

HCID 86628515N-(2,6-difluoropyridin-3-yl)formamide

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 15413tert-Butyl methyl ether溶媒

実験手順

Acetic anhydride (6 ml) was added to formic acid (6 ml), followed by stirring at room temperature for 20 minutes. Then, a solution of 2,6-difluoro-3-aminopyridine (2.06 g) in tert-butyl methyl ether (7 ml) was added so that the reaction solution was maintained at room temperature. The reaction solution was further stirred at room temperature for four hours. Ethyl acetate and a saturated sodium bicarbonate solution were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and then the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (2.42 g). The property values of the compound are as follows.

後処理

  1. temperaturewas maintained at room temperature
  2. stirringThe reaction solution was further stirred at room temperature for four hours
  3. customthe organic layer was separated
  4. washThe resulting organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe drying agent was separated by filtration
  7. concentrationthe organic layer was concentrated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-baa37e6433c247bc9d522fbb5ae9a100
出典データセット
uspto-grants-2011_05
特許番号
US07935815B2

反応ノート

読み込み中…