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

HRID 392329

反応式

HRID 392329 の反応式
[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

参加物

5

反応物 2

HCID 22662794Methyl 3-methoxy-6-nitro-2-pyrazinecarboxylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22662843Methyl 6-amino-3-methoxy-2-pyrazinecarboxylate収率 71.8%

試薬・触媒・溶媒 2

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d607e4676fc845f4bdd82f325eb24bc2
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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