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HCID 19008600, 화합물 → HCID 19008596, 화합물

HRID 1742186
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HRID 1742186 반응식
[Cl:1][C:2]1[CH:29]=[C:28]([C:30]([F:33])([F:32])[F:31])[CH:27]=[CH:26][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:23]([O-])=O)=[C:9]([CH:22]=1)[O:10][CH:11]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:12]([O:14]CC)=O>C(O)C.[Ni]>[Cl:1][C:2]1[CH:29]=[C:28]([C:30]([F:31])([F:33])[F:32])[CH:27]=[CH:26][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]2[NH:23][C:12](=[O:14])[CH:11]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[O:10][C:9]=2[CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 19008600HCID 19008600, 화합물

생성물 1

HCID 19008596HCID 19008596, 화합물수율 53.2%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

Diethyl 2-[5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrophenoxy]malonate (Reference compound IV-1) (2.0 g) was dissolved in ethanol (20 ml), and a hydrogenation was carried out, with addition of Raney nickel as the catalyst, at room temperature under normal pressure for 10 hours. The reaction mixture was filtered, the filtrate concentrated under a reduced pressure, and the residue obtained was purified by silica gel chromatography (eluant: n-hexane/ethyl acetate=3/1) to give 0.9 g of the title compound (colorless crystals).

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate concentrated under a reduced pressure
  3. customthe residue obtained
  4. customwas purified by silica gel chromatography (eluant: n-hexane/ethyl acetate=3/1)

출처 및 근거

ORD 기록
ord-12b2433b941142f2a48e759cd3b9bdce
출처 데이터셋
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05338719

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