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2-(2-Chloro-4-fluorophenyl)-3-methyl-5-nitropyridine → 6-(2-Chloro-4-fluorophenyl)-5-methylpyridin-3-amine

HRID 394174
ノート
印刷プレビュー

反応式

HRID 394174 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:14]([CH3:15])=[CH:13][C:12]([N+:16]([O-])=O)=[CH:11][N:10]=1>[Ni].CO.CO>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:10]=[CH:11][C:12]([NH2:16])=[CH:13][C:14]=1[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 226479942-(2-Chloro-4-fluorophenyl)-3-methyl-5-nitropyridine

生成物 1

HCID 226481546-(2-Chloro-4-fluorophenyl)-5-methylpyridin-3-amine

試薬・触媒・溶媒 2

HCID 22477019Nickel monomethoxide触媒HCID 887Methanol溶媒

実験手順

A 250 mL round bottom flask was charged with 2-(2-chloro-4-fluorophenyl)-3-methyl-5-nitropyridine (4 g) and methanol (50 mL). To the flask was added Raney nickel/methanol slurry (approx 4 g). The flask was evacuated and charged with hydrogen several times. The mixture was stirred under a balloon of hydrogen for 2.5 h. The flask was purged with nitrogen. The catalyst was filtered off and the filtrate was concentrated under reduced pressure giving 6-(2-chloro-4-fluorophenyl)-5-methylpyridin-3-amine as an off white solid. Mass spectrum (EST) 237 (M+1).

後処理

  1. customThe flask was evacuated
  2. additioncharged with hydrogen several times
  3. customThe flask was purged with nitrogen
  4. filtrationThe catalyst was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-fa1e18fe8b434a2daf01a9b5e4b920b4
出典データセット
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06809199B2

反応ノート

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