2-Chloro-3-nitropyridine → N-(4-methoxybutyl)-3-nitropyridin-2-amine

HRID 1259918노트

반응식

HRID 1259918 반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.Cl.[CH3:12][O:13][CH2:14][CH2:15][CH2:16][CH2:17][NH2:18].C(N(C(C)C)CC)(C)C>CC(O)C>[CH3:12][O:13][CH2:14][CH2:15][CH2:16][CH2:17][NH:18][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 796132-Chloro-3-nitropyridineHCID 81531DiisopropylethylamineHCID 457923494-Methoxybutan-1-amine hydrochloride

생성물 1

HCID 58355169N-(4-methoxybutyl)-3-nitropyridin-2-amine수율 84.7%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

2-Chloro-3-nitropyridine (3.54 g) and 4-methoxybutan-1-amine hydrochloride (3.12 g) were suspended in 2-propanol (100 ml), diisopropylethylamine (11.6 μl) was added and the mixture was heated under reflux with stirring for 4 days. The reaction mixture was cooled to room temperature, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate-hexane (3:7) was concentrated under reduced pressure to give the object product (4.26 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. concentrationconcentrated under reduced pressure
  4. washa fraction eluted with ethyl acetate-hexane (3:7)
  5. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-cd76cf4058864dad883bc2b3b9d2635a
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466282B2

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