Methyl 3-methoxy-6-nitro-2-pyrazinecarboxylate → Methyl 6-amino-3-methoxy-2-pyrazinecarboxylate

HRID 392329

반응식

HRID 392329 반응식
[H][H].[CH3:3][O:4][C:5]1[C:6]([C:14]([O:16][CH3:17])=[O:15])=[N:7][C:8]([N+:11]([O-])=O)=[CH:9][N:10]=1>C(=O)([O-])[O-].[Ca+2].[Pd+2].C(=O)([O-])[O-].C(O)(=O)C>[NH2:11][C:8]1[N:7]=[C:6]([C:14]([O:16][CH3:17])=[O:15])[C:5]([O:4][CH3:3])=[N:10][CH:9]=1

참가 물질

5

반응물 2

HCID 22662794Methyl 3-methoxy-6-nitro-2-pyrazinecarboxylateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22662843Methyl 6-amino-3-methoxy-2-pyrazinecarboxylate수율 71.8%

시약·촉매·용매 2

HCID 17803853Palladium on calcium carbonate촉매HCID 176Acetic Acid용매

실험 절차

At room temperature and under a pressure of 1 atmosphere, hydrogen gas was introduced into a mixture of 24.3 g of methyl 3-methoxy-6-nitro-2-pyrazinecarboxylate, 480 mL of acetic acid and 1.2 g of lead-poisoned palladium-calcium carbonate until the mixture became showing no further absorption of hydrogen. After filtering off insoluble matter from the reaction mixture, the solvent was removed under reduced pressure, and the solid product thus obtained was washed with ethyl acetate and diethyl ether. Thus, 15.0 g of methyl 6-amino-3-metoxy-2-pyrazinecarboxylate was obtained as a solid product. Furthermore, the solvent was removed from the filtrate under reduced pressure to obtain a solid product, and the solid product was washed with ethyl acetate to obtain 2.3 g of methyl 6-amino-3-methoxy-2-pyrazinecarboxylate as a solid product.

후처리

  1. customno further absorption of hydrogen
  2. filtrationAfter filtering off insoluble matter from the reaction mixture
  3. customthe solvent was removed under reduced pressure
  4. customthe solid product thus obtained
  5. washwas washed with ethyl acetate and diethyl ether

출처 및 근거

ORD 기록
ord-d607e4676fc845f4bdd82f325eb24bc2
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06800629B2

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