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

HRID 37493
ノート
印刷プレビュー

反応式

HRID 37493 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fc02068cd0c1425ea5a7e41355468849
出典データセット
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05420275

反応ノート

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