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

HRID 1259951ノート

反応式

HRID 1259951 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-cc0689c478bf4f628aff55a3cdde54da
出典データセット
uspto-grants-2013_06
特許番号
US08466282B2

反応ノート

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