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

HRID 1644586노트

반응식

HRID 1644586 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

HCID 22387769Ethyl 6-amino-5-nitropyridine-3-carboxylate수율 73%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0a933b6db7ba42edaa12b86b107ed684
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08124617B2

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