Ethanol → Ethyl 6-amino-5-nitropyridine-3-carboxylate

HRID 1644586ノート

反応式

HRID 1644586 の反応式
[NH2:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1.S(=O)(=O)(O)O.[CH2:19](O)[CH3:20]>>[NH2:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([O:8][CH2:19][CH3:20])=[O:7])=[CH:4][N:3]=1

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 2718816-Amino-5-nitronicotinic acid

生成物 1

HCID 22387769Ethyl 6-amino-5-nitropyridine-3-carboxylate収率 73%

実験手順

A solution of 6-amino-5-nitronicotinic acid (10 g) and concentrated sulfuric acid (20 ml) in ethanol (250 ml) was heated under reflux for 18 hr. The reaction mixture was concentrated, diluted with water and adjusted with sodium hydrogencarbonate to pH 8. The precipitated crystals were collected by filtration and washed with water to give the title compound (8.5 g, yield 73%) as yellow crystals. purity 84%. M+H: 212.

後処理

  1. temperatureunder reflux for 18 hr
  2. concentrationThe reaction mixture was concentrated
  3. additiondiluted with water
  4. filtrationThe precipitated crystals were collected by filtration
  5. washwashed with water

出典と根拠

ORDレコード
ord-0a933b6db7ba42edaa12b86b107ed684
出典データセット
uspto-grants-2012_02
特許番号
US08124617B2

反応ノート

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