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

HRID 1509463
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HRID 1509463 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-bb37099e95634b35b72e3e3731f2d35d
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09221836B2

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