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Hydrazine hydrate (1:1) → HCID 178419935, 화합물

HRID 34011
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반응식

HRID 34011 반응식
Cl[C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([C:9]1[CH:18]=[CH:17][C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:10]=1)=O.O.[NH2:20][NH2:21]>C(O)C.C(OCC)(=O)C>[CH:10]1[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:17]=[CH:18][C:9]=1[C:7]1[C:6]2[CH:5]=[CH:4][S:3][C:2]=2[NH:20][N:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 23070192(2-Chlorothiophen-3-yl)-(naphthalen-2-yl)-methanone

생성물 1

HCID 178419935HCID 178419935, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 0.61 g of (2-chlorothiophen-3-yl)-(naphthalen-2-yl)-methanone in 6 mL of ethanol was added 0.12 mL of hydrazine monohydrate at room temperature and heated under reflux for 2 days. The reaction solution was diluted with ethyl acetate, and the organic layer washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The resultant crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30-1:5), to afford 32 mg of the title compound as colorless crystals.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 2 days
  3. washthe organic layer washed successively with saturated aqueous ammonium chloride and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated
  6. customThe resultant crude product was purified
  7. customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:30-1:5)

출처 및 근거

ORD 기록
ord-be84753c31034ea4b8b82e9f385d878d
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07429609B2

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