Acetic Acid → 3-Amino-6-chloropyridine-2-carbonitrile

HRID 1517427ノート

反応式

HRID 1517427 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([C:8]#[N:9])[C:5]([N+:10]([O-])=O)=[CH:4][CH:3]=1.C(O)(=O)C.[O-]S(S([O-])=O)=O.[Na+].[Na+].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O>[NH2:10][C:5]1[C:6]([C:8]#[N:9])=[N:7][C:2]([Cl:1])=[CH:3][CH:4]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 14812Phosphorus oxide (P4O10)HCID 24489Sodium DithioniteHCID 133817056-Chloro-3-nitropyridine-2-carbonitrile

生成物 1

HCID 5927503-Amino-6-chloropyridine-2-carbonitrile収率 80.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a suspension of 6-chloro-3-nitro-pyridine-2-carbonitrile (5.5 g, 30 mmol) in water (100 ml), was added acetic acid (5.4 ml, 90 mmol). The mixture was stirred at room temperature for 20 minutes. Then, Na2S2O4 (20 g, 86%, 90 mmol) was added slowly. The reaction mixture was stirred at room temperature for another 2 hours. The precipitate was filtered off and washed with cold water (2×10 ml). The precipitate was dried over P2O5 yielding the title compound as a yellowish solid (3.7 g, yield: 80%) which was characterised as follows:

後処理

  1. stirringThe reaction mixture was stirred at room temperature for another 2 hours
  2. filtrationThe precipitate was filtered off
  3. washwashed with cold water (2×10 ml)

出典と根拠

ORDレコード
ord-35e062a7687e45758a82e9a06f4508d2
出典データセット
uspto-grants-2012_07
特許番号
US08232278B2

反応ノート

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