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Stannous chloride dihydrate → HCID 57438891, 화합물

HRID 1669776
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HRID 1669776 반응식
[CH3:1][C:2]1[O:3][C:4]2[C:9]([C:10](=[O:12])[CH:11]=1)=[C:8]([N+:13]([O-])=O)[CH:7]=[CH:6][C:5]=2[CH3:16].O.O.[Sn](Cl)Cl.C(=O)(O)[O-].[Na+]>C(OCC)(=O)C>[NH2:13][C:8]1[CH:7]=[CH:6][C:5]([CH3:16])=[C:4]2[C:9]=1[C:10](=[O:12])[CH:11]=[C:2]([CH3:1])[O:3]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 574388902,8-Dimethyl-5-nitro-4H-chromen-4-one

생성물 1

HCID 57438891HCID 57438891, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

1.78 g (8.12 mmol) of 2,8-dimethyl-5-nitro-4H-chromen-4-one are heated with 9.16 g (40.6 mmol) of tin(II) chloride dihydrate in 70 ml of ethyl acetate at 70° C. overnight. After cooling to room temperature, the reaction mixture is brought to pH 9-10 with saturated sodium bicarbonate solution. After filtration through kieselguhr, the organic phase is separated off, and the aqueous phase is extracted several times with ethyl acetate. The combined organic phases are washed with saturated sodium chloride solution. After drying over sodium sulfate, the solvent is removed in vacuo. 1.5 g (99% of theory) of the title compound are obtained.

후처리

  1. filtrationAfter filtration through kieselguhr
  2. customthe organic phase is separated off
  3. extractionthe aqueous phase is extracted several times with ethyl acetate
  4. washThe combined organic phases are washed with saturated sodium chloride solution
  5. dry with materialAfter drying over sodium sulfate
  6. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-f3da7ac5975b464eb4377534605cc6ac
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989633B2

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