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Hydrogen chloride-ethyl acetate → 3-methoxy-N-(4-methoxybutyl)-2-nitroaniline

HRID 1509463
ノート
印刷プレビュー

反応式

HRID 1509463 の反応式
C(OC(=O)[N:7]([CH2:19][CH2:20][CH2:21][CH2:22][O:23][CH3:24])[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[C:9]=1[N+:16]([O-:18])=[O:17])(C)(C)C.C(OCC)(=O)C.Cl>C(OCC)(=O)C>[CH3:15][O:14][C:10]1[C:9]([N+:16]([O-:18])=[O:17])=[C:8]([CH:13]=[CH:12][CH:11]=1)[NH:7][CH2:19][CH2:20][CH2:21][CH2:22][O:23][CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 58355557Tert-butyl (4-methoxybutyl)(3-methoxy-2-nitrophenyl)carbamate

生成物 1

HCID 583557683-methoxy-N-(4-methoxybutyl)-2-nitroaniline収率 99.1%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

tert-Butyl(4-methoxybutyl)(3-methoxy-2-nitrophenyl)carbamate (2.11 g) was dissolved in ethyl acetate (30 ml), 4M hydrogen chloride-ethyl acetate (15 ml) was added, and the mixture was stirred for 12 hr. The reaction mixture was concentrated under reduced pressure, diluted with saturated aqueous sodium hydrogen carbonate, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, concentration under reduced pressure to give the object product (1.50 g).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additiondiluted with saturated aqueous sodium hydrogen carbonate
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate, concentration under reduced pressure

出典と根拠

ORDレコード
ord-bb37099e95634b35b72e3e3731f2d35d
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09221836B2

反応ノート

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