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

HRID 1184130ノート

反応式

HRID 1184130 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7d50255b757f41c480f65c04128b212a
出典データセット
uspto-grants-2014_03
特許番号
US08664380B2

反応ノート

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