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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → HCID 14722317, 화합물

HRID 1031668
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HRID 1031668 반응식
[CH3:1][O:2][CH:3]1[C:8](=[O:9])[C:7]2[CH:10]=[C:11]([O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:12]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:13][C:6]=2[O:5][CH2:4]1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>O1CCOCC1>[CH3:1][O:2][C:3]1[C:8](=[O:9])[C:7]2[CH:10]=[C:11]([O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:12]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:13][C:6]=2[O:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 14722453HCID 14722453, 화합물

생성물 1

HCID 14722317HCID 14722317, 화합물수율 52.9%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

There were mixed 3.63 g of 2,3-dihydro-3-methoxy-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran4-one, 3.41 g of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone and 150 ml of dioxane. The mixture was refluxed for 48 hours. The reaction mixture was cooled. The resulting precipitate was removed by filtration. The solvent was removed by distillation under reduced pressure. The residue was purified by a column chromatography (eluant: a 3 : 1 mixture of toluene and ethyl acetate) to obtain 1.91 g (yield: 52.9%) of 3-methoxy-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one [Compound No. 2].

후처리

  1. temperatureThe mixture was refluxed for 48 hours
  2. temperatureThe reaction mixture was cooled
  3. customThe resulting precipitate was removed by filtration
  4. customThe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by a column chromatography (eluant
  6. additiona 3 : 1 mixture of toluene and ethyl acetate)

출처 및 근거

ORD 기록
ord-d28791e6ede9425e88289421b912d920
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04954518

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