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

HRID 392353

반응식

HRID 392353 반응식
[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

참가 물질

5

반응물 2

HCID 22662836Methyl 6-fluoro-3-nitro-2-pyrazinecarboxylateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22662844Methyl 3-amino-6-fluoropyrazine-2-carboxylate수율 11.8%

시약·촉매·용매 2

HCID 17803853Palladium on calcium carbonate촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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]

출처 및 근거

ORD 기록
ord-27d2ce7a66aa4c38ae6390899a0cf153
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06800629B2

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