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Water → HCID 59403300, 화합물

HRID 1873865
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HRID 1873865 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1/[CH:9]=[C:10](/[N+:12]([O-:14])=[O:13])\[CH3:11].Cl.[CH3:16][O:17][NH2:18].C(N(CC)CC)C.O>CO>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([NH:18][O:17][CH3:16])[CH:10]([N+:12]([O-:14])=[O:13])[CH3:11]
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참가 물질

6

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HCID 962WaterHCID 8471TriethylamineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 2063266HCID 2063266, 화합물

생성물 1

HCID 59403300HCID 59403300, 화합물수율 82.4%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

To a stirred yellow solution of the 2,4-dichloro-1-((E)-2-nitro-propenyl)-benzene (1.0 mmol, 0.232 g), in methanol (3 ml) under N2 was added at 0° C. O-methylhydroxylamine hydrochloride (2.0 mmol, 0.167 g) and triethylamine (3.0 mmol, 0.30 g). After stirring for 0.5 h at 50° C., the colourless liquid cooled to ambient temperature and water (20 ml) was added. The aqueous solution was extracted with dichloromethane (20 ml), the organic layers were combined, dried (MgSO4), filtered, and evaporated under reduced pressure to afford 0.23 g (82.4% of theory) of N-[1-(2,4-dichloro-phenyl)-2-nitro-propyl]-O-methyl-hydroxylamine in the form of liquid, as a mixture of diastereomeres.

후처리

  1. temperaturethe colourless liquid cooled to ambient temperature
  2. extractionThe aqueous solution was extracted with dichloromethane (20 ml)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-e49f27e3dc004eda80b8a42ff7c4c6fc
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08304444B2

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