Methyl 6-fluoro-3-nitro-2-pyrazinecarboxylate → Methyl 3-amino-6-fluoropyrazine-2-carboxylate

HRID 392353

反応式

HRID 392353 の反応式
[F:1][C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[C:5]([N+:12]([O-])=O)=[N:4][CH:3]=1.[H][H]>C(O)(=O)C.C(=O)([O-])[O-].[Ca+2].[Pd+2].C(=O)([O-])[O-]>[NH2:12][C:5]1[C:6]([C:8]([O:10][CH3:11])=[O:9])=[N:7][C:2]([F:1])=[CH:3][N:4]=1

参加物

5

反応物 2

HCID 22662836Methyl 6-fluoro-3-nitro-2-pyrazinecarboxylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22662844Methyl 3-amino-6-fluoropyrazine-2-carboxylate収率 11.8%

試薬・触媒・溶媒 2

HCID 17803853Palladium on calcium carbonate触媒HCID 176Acetic Acid溶媒

実験手順

In 1.0 mL of acetic acid was dissolved 20 mg of methyl 6-fluoro-3-nitro-2-pyrazinecarboxylate. After adding 6 mg of lead-poisoned palladium-calcium carbonate, hydrogen gas was introduced into the mixture at room temperature under a pressure of 1 atmosphere, until the mixture became absorbing no further quantity of hydrogen gas. The insoluble matter was filtered off from the reaction mixture, and the filtrate was concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=5:1] to obtain 2 mg of methyl 3-amino-6-fluoro-2-pyrazinecarboxylate as a light yellow-colored solid product.

後処理

  1. additionwas introduced into the mixture at room temperature under a pressure of 1 atmosphere, until the mixture
  2. custombecame absorbing no further quantity of hydrogen gas
  3. filtrationThe insoluble matter was filtered off from the reaction mixture
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue thus obtained
  6. customwas purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=5:1]

出典と根拠

ORDレコード
ord-27d2ce7a66aa4c38ae6390899a0cf153
出典データセット
uspto-grants-2004_10
特許番号
US06800629B2

関連ノート

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