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Stannous chloride dihydrate → HCID 57438891、化合物

HRID 557429
ノート
印刷プレビュー

反応式

HRID 557429 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 57438891HCID 57438891、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

1.78 g (8.12 mmol) of 2,8-dimethyl-5-nitro-4H-chromen-4-one (example 32, stage c) 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 adjusted 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.

後処理

  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

出典と根拠

ORDレコード
ord-3d5407f7b9294658a555e90b14795492
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058447B2

反応ノート

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