Hydrochloric Acid → HCID 118598586、化合物

HRID 1050364ノート

反応式

HRID 1050364 の反応式
[F:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4](C(OC)=O)[CH:3]=1.OO.NC(N)=[O:16].FC(F)(F)[C:20]([O:22][C:23](=[O:28])[C:24](F)(F)F)=O.Cl>ClCCl>[CH3:4][C:3]1[C:24]([C:23]([O:22][CH3:20])=[O:28])=[N+:5]([O-:16])[CH:6]=[CH:7][C:2]=1[F:1]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 9845Trifluoroacetic anhydrideHCID 31294Carbamide PeroxideHCID 46311149Methyl 4-fluoropyridine-2-carboxylate

生成物 1

HCID 118598586HCID 118598586、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of methyl 4-fluoropicolinate (2, 1 g, 6.45 mmol) in dichloromethane (30 mL) is added urea hydrogen peroxide (1.27 g, 13.54 mmol) and trifluoroacetic anhydride (1.79 mL, 12.9 mmol). The reaction is stirred at room temperature for 2 h. The resulting mixture is pour into 0.5 M hydrochloric acid and extracted with dichloromethane. The organic layer is washed with saturated aqueous sodium bicarbonate solution, dried over magnesium sulfate, filtered and concentrated. The crude is purified via flash chromatography to afford methyl 4-fluoro-2-(methoxycarbonyl)pyridine 1-oxide (3).

後処理

  1. extractionextracted with dichloromethane
  2. washThe organic layer is washed with saturated aqueous sodium bicarbonate solution
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude is purified via flash chromatography

出典と根拠

ORDレコード
ord-d2f6dd8838264e709ed51b842c805886
出典データセット
uspto-grants-2016_07
特許番号
US09382248B2

反応ノート

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