Diisopropylethylamine → 3-fluoro-N-(4-methoxybutyl)-2-nitroaniline

HRID 1184130노트

반응식

HRID 1184130 반응식
F[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N+:9]([O-:11])=[O:10].C(N(C(C)C)CC)(C)C.Cl.[CH3:22][O:23][CH2:24][CH2:25][CH2:26][CH2:27][NH2:28]>C(#N)C>[F:8][C:4]1[C:3]([N+:9]([O-:11])=[O:10])=[C:2]([CH:7]=[CH:6][CH:5]=1)[NH:28][CH2:27][CH2:26][CH2:25][CH2:24][O:23][CH3:22]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 879221,3-Difluoro-2-nitrobenzeneHCID 457923494-Methoxybutan-1-amine hydrochloride

생성물 1

HCID 583554133-fluoro-N-(4-methoxybutyl)-2-nitroaniline수율 66.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To a solution of 1,3-difluoro-2-nitrobenzene (3.00 g) and diisopropylethylamine (7 μl) in acetonitrile (30 ml) was added a solution of 4-methoxybutan-1-amine hydrochloride (2.51 g) in acetonitrile (10 ml), and the mixture was stirred at room temperature for 90 hr. The reaction mixture was concentrated under reduced pressure, and the residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate-hexane (2:98-25:75) was concentrated under reduced pressure to give the object product (2.90 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. washa fraction eluted with ethyl acetate-hexane (2:98-25:75)
  3. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7d50255b757f41c480f65c04128b212a
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08664380B2

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