2-Methyl-5-methylamino-6-nitro-pyridine → HCID 18412465、化合物

HRID 2227623ノート

反応式

HRID 2227623 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH3:9])=[C:4]([N+:10]([O-])=O)[N:3]=1>C(OCC)(=O)C.[Ni]>[NH2:10][C:4]1[C:5]([NH:8][CH3:9])=[CH:6][CH:7]=[C:2]([CH3:1])[N:3]=1

参加物

4

反応物 1

HCID 149295782-Methyl-5-methylamino-6-nitro-pyridine

生成物 1

HCID 18412465HCID 18412465、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8857Ethyl Acetate溶媒

実験手順

8.35 g (50 mmol) of 2-Methyl-5-methylamino-6-nitropyridine (Heterocycles 38, 529 (1994)) were dissolved in 300 l ethyl acetate and hydrogenated with 1.5 g Raney nickel for 3.5 hours at room temperature. Then the catalyst was filtered off and the filtrate was evaporated down. After crystallization of the resulting residue from petroleum ether, 5.75 g (84% of theory) were obtained as olive-green crystals. C7H11N3 (137.20). Melting point: 112-113° C.

後処理

  1. filtrationThen the catalyst was filtered off
  2. customthe filtrate was evaporated down
  3. customAfter crystallization of the resulting residue from petroleum ether
  4. custom5.75 g (84% of theory) were obtained as olive-green crystals

出典と根拠

ORDレコード
ord-6b89f5081e4f438187fbfbf24fc0da0c
出典データセット
uspto-grants-2002_07
特許番号
US06414008B1

反応ノート

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