Hydrochloric Acid → HCID 118598586, 화합물

HRID 1050364노트

반응식

HRID 1050364 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 118598586HCID 118598586, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d2f6dd8838264e709ed51b842c805886
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09382248B2

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