Potassium Carbonate → HCID 178498306, 화합물

HRID 1251915노트

반응식

HRID 1251915 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][CH:11]=[CH:10][N+:9]=2[O-])=[CH:4][CH:3]=1.C(=O)([O-])[O-:20].[K+].[K+]>C(OC(=O)C)(=O)C.CO.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][CH:11]=[C:10]([OH:20])[N:9]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 2

HCID 11430Potassium CarbonateHCID 183245012-(4-Fluorophenyl)-3-(methoxycarbonyl)pyridine-1-oxide

생성물 1

HCID 178498306HCID 178498306, 화합물수율 76.2%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 7918Acetic Anhydride용매

실험 절차

A solution of 2-(4-fluorophenyl)-3-(methoxycarbonyl)pyridine-1-oxide (10.5 g.) in acetic anhydride (500 ml.) was stirred at reflux for 17 hr., cooled, evaporated to dryness and the residue partitioned between saturated sodium bicarbonate solution and ethyl acetate. The organic layer was separated, dried and evaporated to dryness. The gum obtained was dissolved in methanol (400 ml.), treated with a solution of potassium carbonate (11.7 g.) in water (100 ml) and stirred at ambient temperature for 2 hours. The methanol was evaporated off, the aqueous residue diluted with more water (200 ml.) and the mixture filtered to give methyl 2-(4-fluorophenyl)-6-hydroxypyridin-3-carboxylate (8.0 g.) as a brown solid.

후처리

  1. temperatureat reflux for 17 hr
  2. temperature, cooled
  3. customevaporated to dryness
  4. customthe residue partitioned between saturated sodium bicarbonate solution and ethyl acetate
  5. customThe organic layer was separated
  6. customdried
  7. customevaporated to dryness
  8. customThe gum obtained
  9. customThe methanol was evaporated off
  10. additionthe aqueous residue diluted with more water (200 ml.)
  11. filtrationthe mixture filtered

출처 및 근거

ORD 기록
ord-c10c598bafa443a9814c801f8a285ca6
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06342765B1

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