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Acetic Acid → 3-Amino-6-fluoro-4,5-diethoxycarbonyl-2-phenylpyridine

HRID 37493
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HRID 37493 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:7]([F:26])=[N:8][C:9]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[C:10]([N+:17]([O-])=O)[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:5])[CH3:2].C(O)(=O)C>C(O)C>[NH2:17][C:10]1[C:9]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)=[N:8][C:7]([F:26])=[C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 199356173,4-Diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine

생성물 1

HCID 152896983-Amino-6-fluoro-4,5-diethoxycarbonyl-2-phenylpyridine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In 5 ml of ethanol was dissolved 160 mg of 3,4-diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine, and 120 mg (5 eq.) of reduced iron was added to the solution, followed by addition of 0.5 ml (20 eq.) of acetic acid. After the mixture was refluxed for 30 minutes, the solvent was distilled off. The residue was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the precipitate was removed by filtration, the obtained organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. Then, the solvent was distilled off.

후처리

  1. additionwas added to the solution
  2. temperatureAfter the mixture was refluxed for 30 minutes
  3. distillationthe solvent was distilled off
  4. extractionfollowed by extraction with ethyl acetate
  5. customAfter the precipitate was removed by filtration
  6. washthe obtained organic layer was washed with water
  7. dry with materiala saturated aqueous solution of sodium chloride, and dried
  8. distillationThen, the solvent was distilled off

출처 및 근거

ORD 기록
ord-fc02068cd0c1425ea5a7e41355468849
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05420275

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